 
data_shelx
 
_audit_creation_method            SHELXL-2014
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C27 H32 N10 Ni O10 W Y' 
_chemical_formula_weight          988.09

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni'  'Ni'   0.3393   1.1124
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Y'  'Y'  -2.7962   3.5667
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    8.9506(5)
_cell_length_b                    13.9237(6)
_cell_length_c                    27.4023(15)
_cell_angle_alpha                 90
_cell_angle_beta                  93.252(4)
_cell_angle_gamma                 90
_cell_volume                      3409.5(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     57563 
_cell_measurement_theta_min       2.08 
_cell_measurement_theta_max       32.63 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             green 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.925          
_exptl_crystal_F_000              1940
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.5 
_exptl_crystal_size_mid           0.3 
_exptl_crystal_size_min           0.2 
_exptl_absorpt_coefficient_mu     5.669
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.1450 
_exptl_absorpt_correction_T_max   0.3411 
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                       
_diffrn_measurement_device_type   'STOE-IPDS II' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             31808
_diffrn_reflns_av_unetI/netI      0.0641
_diffrn_reflns_av_R_equivalents   0.0932
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -36
_diffrn_reflns_limit_l_max        36
_diffrn_reflns_theta_min          2.670
_diffrn_reflns_theta_max          27.999
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.997
_diffrn_measured_fraction_theta_full  0.996
_diffrn_reflns_Laue_measured_fraction_max    0.997
_diffrn_reflns_Laue_measured_fraction_full   0.996
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.996
_reflns_number_total              8193
_reflns_number_gt                 6327
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'X-Area'
_computing_cell_refinement        'X-Area'
_computing_data_reduction         'X-Area'
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0482P)²+20.7845P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00070(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          8193
_refine_ls_number_parameters      452
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0840
_refine_ls_R_factor_gt            0.0597
_refine_ls_wR_factor_ref          0.1399
_refine_ls_wR_factor_gt           0.1264
_refine_ls_goodness_of_fit_ref    1.064
_refine_ls_restrained_S_all       1.064
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.6513(14) 0.3353(11) 0.0222(4) 0.075(4) Uani 1 1 d . . . . .
H1A H 0.6016 0.2886 0.0012 0.112 Uiso 1 1 calc R U . . .
H1B H 0.6652 0.3935 0.0043 0.112 Uiso 1 1 calc R U . . .
H1C H 0.7469 0.3107 0.0340 0.112 Uiso 1 1 calc R U . . .
O9 O 0.2993(7) 0.2636(4) 0.2275(2) 0.0416(13) Uani 1 1 d . . . . .
C2 C 0.6192(10) 0.4219(7) 0.0971(3) 0.0410(18) Uani 1 1 d . . . . .
C3 C 0.7435(12) 0.4792(8) 0.0904(4) 0.056(3) Uani 1 1 d . . . . .
H3 H 0.7939 0.4755 0.0618 0.067 Uiso 1 1 calc R U . . .
C4 C 0.7900(12) 0.5412(9) 0.1269(4) 0.063(3) Uani 1 1 d . . . . .
H4 H 0.8723 0.5805 0.1227 0.075 Uiso 1 1 calc R U . . .
C5 C 0.7171(12) 0.5464(8) 0.1696(4) 0.060(3) Uani 1 1 d . . . . .
H5 H 0.7527 0.5875 0.1944 0.072 Uiso 1 1 calc R U . . .
C6 C 0.5901(11) 0.4908(6) 0.1762(3) 0.0437(19) Uani 1 1 d . . . . .
C7 C 0.5398(9) 0.4257(6) 0.1394(3) 0.0375(17) Uani 1 1 d . . . . .
C8 C 0.5170(12) 0.5032(7) 0.2222(3) 0.049(2) Uani 1 1 d . . . . .
H8 H 0.5704 0.5382 0.2463 0.059 Uiso 1 1 calc R U . . .
C9 C 0.3383(14) 0.5056(9) 0.2810(4) 0.066(3) Uani 1 1 d . . . . .
H9A H 0.4159 0.4914 0.3062 0.079 Uiso 1 1 calc R U . . .
H9B H 0.3268 0.5748 0.2797 0.079 Uiso 1 1 calc R U . . .
C10 C 0.1992(17) 0.4641(10) 0.2956(4) 0.079(4) Uani 1 1 d . . . . .
H10A H 0.1778 0.4907 0.3272 0.095 Uiso 1 1 calc R U . . .
H10B H 0.2142 0.3956 0.3000 0.095 Uiso 1 1 calc R U . . .
C11 C 0.0629(15) 0.4786(9) 0.2613(4) 0.067(3) Uani 1 1 d . . . . .
H11A H -0.0263 0.4688 0.2792 0.080 Uiso 1 1 calc R U . . .
H11B H 0.0616 0.5443 0.2496 0.080 Uiso 1 1 calc R U . . .
C12 C -0.0583(11) 0.3655(7) 0.2093(3) 0.050(2) Uani 1 1 d . . . . .
H12 H -0.1383 0.3766 0.2288 0.060 Uiso 1 1 calc R U . . .
C13 C -0.0822(10) 0.2951(7) 0.1704(3) 0.0430(19) Uani 1 1 d . . . . .
C14 C -0.2203(10) 0.2473(8) 0.1678(3) 0.050(2) Uani 1 1 d . . . . .
H14 H -0.2907 0.2625 0.1903 0.060 Uiso 1 1 calc R U . . .
C15 C -0.2543(12) 0.1786(9) 0.1331(4) 0.062(3) Uani 1 1 d . . . . .
H15 H -0.3466 0.1478 0.1325 0.075 Uiso 1 1 calc R U . . .
C16 C -0.1518(11) 0.1546(8) 0.0988(4) 0.054(2) Uani 1 1 d . . . . .
H16 H -0.1744 0.1084 0.0750 0.065 Uiso 1 1 calc R U . . .
C17 C -0.0152(10) 0.2015(7) 0.1010(3) 0.045(2) Uani 1 1 d . . . . .
C18 C 0.0215(9) 0.2730(6) 0.1360(3) 0.0387(18) Uani 1 1 d . . . . .
C19 C 0.0833(15) 0.0967(8) 0.0409(4) 0.069(3) Uani 1 1 d . . . . .
H19A H 0.1657 0.0915 0.0201 0.104 Uiso 1 1 calc R U . . .
H19B H 0.0837 0.0426 0.0627 0.104 Uiso 1 1 calc R U . . .
H19C H -0.0090 0.0977 0.0213 0.104 Uiso 1 1 calc R U . . .
C20 C 0.2043(9) 0.6086(6) 0.1383(3) 0.0376(17) Uani 1 1 d . . . . .
C21 C 0.0779(10) 0.6757(7) 0.0618(3) 0.0437(19) Uani 1 1 d . . . . .
C27 C 0.3348(10) 0.7501(7) 0.1865(3) 0.0423(19) Uani 1 1 d . . . . .
C22 C 0.0311(9) 0.7388(6) 0.1772(3) 0.0369(16) Uani 1 1 d . . . . .
N10 N 0.4170(10) 0.7475(7) 0.2192(3) 0.057(2) Uani 1 1 d . . . . .
C23 C -0.0152(11) 0.8373(7) 0.0998(3) 0.046(2) Uani 1 1 d . . . . .
C24 C 0.2342(12) 0.9028(6) 0.1477(3) 0.047(2) Uani 1 1 d . . . . .
C25 C 0.2342(12) 0.8435(6) 0.0564(3) 0.044(2) Uani 1 1 d . . . . .
C26 C 0.4067(10) 0.7223(8) 0.0966(3) 0.051(2) Uani 1 1 d . . . . .
N1 N 0.3898(9) 0.4723(5) 0.2334(2) 0.0433(17) Uani 1 1 d . . . . .
N2 N 0.0596(8) 0.4133(6) 0.2196(2) 0.0417(16) Uani 1 1 d . . . . .
N3 N 0.2159(9) 0.5293(5) 0.1475(3) 0.0453(18) Uani 1 1 d . . . . .
N4 N 0.0186(10) 0.6335(7) 0.0314(3) 0.054(2) Uani 1 1 d . . . . .
N5 N -0.0541(9) 0.7280(6) 0.2070(3) 0.0492(18) Uani 1 1 d . . . . .
N6 N -0.1229(11) 0.8776(7) 0.0871(3) 0.065(2) Uani 1 1 d . . . . .
N7 N 0.2645(14) 0.9791(6) 0.1584(4) 0.073(3) Uani 1 1 d . . . . .
N8 N 0.2621(12) 0.8872(7) 0.0233(3) 0.065(3) Uani 1 1 d . . . . .
N9 N 0.5207(11) 0.7109(9) 0.0824(3) 0.078(3) Uani 1 1 d . . . . .
Ni1 Ni 0.25241(12) 0.39916(8) 0.18551(4) 0.0357(2) Uani 1 1 d . . . . .
O1 O 0.5604(7) 0.3550(5) 0.0635(2) 0.0477(15) Uani 1 1 d . . . . .
O2 O 0.4235(7) 0.3679(4) 0.1419(2) 0.0397(13) Uani 1 1 d . . . . .
O3 O 0.1533(6) 0.3156(4) 0.1331(2) 0.0378(12) Uani 1 1 d . . . . .
O4 O 0.0974(7) 0.1845(5) 0.0691(2) 0.0470(15) Uani 1 1 d . . . . .
O5 O 0.2114(9) 0.4208(5) 0.0488(2) 0.0596(19) Uani 1 1 d . . . . .
O6 O 0.2886(7) 0.2709(5) -0.0078(2) 0.0523(16) Uani 1 1 d . . . . .
O7 O 0.4548(9) 0.1382(5) 0.0487(3) 0.063(2) Uani 1 1 d . . . . .
O8 O 0.3660(7) 0.1637(4) 0.1444(2) 0.0428(14) Uani 1 1 d . . . . .
O10 O 0.5880(13) 0.9621(10) 0.0700(8) 0.200(9) Uani 1 1 d . . . . .
W1 W 0.18773(4) 0.75975(2) 0.12089(2) 0.03246(11) Uani 1 1 d . . . . .
Y1 Y 0.32800(9) 0.27482(6) 0.08002(3) 0.03573(18) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.456(11) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
O9 Ni1 2.238(6) . ?
C2 C3 1.390(13) . ?
C2 O1 1.392(10) . ?
C2 C7 1.393(12) . ?
C3 C4 1.367(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.411(12) . ?
C6 C8 1.463(13) . ?
C7 O2 1.320(10) . ?
C8 N1 1.271(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.449(17) . ?
C9 N1 1.482(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.509(18) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.460(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N2 1.266(12) . ?
C12 C13 1.455(13) . ?
C12 H12 0.9300 . ?
C13 C18 1.395(12) . ?
C13 C14 1.402(13) . ?
C14 C15 1.370(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.392(16) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(13) . ?
C16 H16 0.9300 . ?
C17 O4 1.393(11) . ?
C17 C18 1.407(13) . ?
C18 O3 1.327(10) . ?
C19 O4 1.448(11) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N3 1.137(11) . ?
C20 W1 2.160(9) . ?
C21 N4 1.128(11) . ?
C21 W1 2.185(9) . ?
C27 N10 1.127(11) . ?
C27 W1 2.171(7) . ?
C22 N5 1.157(11) . ?
C22 W1 2.164(7) . ?
C23 N6 1.152(13) . ?
C23 W1 2.163(10) . ?
C24 N7 1.131(12) . ?
C24 W1 2.156(9) . ?
C25 N8 1.132(11) . ?
C25 W1 2.178(8) . ?
C26 N9 1.123(12) . ?
C26 W1 2.169(9) . ?
N1 Ni1 2.023(7) . ?
N2 Ni1 2.018(7) . ?
N3 Ni1 2.106(8) . ?
Ni1 O3 2.014(6) . ?
Ni1 O2 2.043(6) . ?
Ni1 Y1 3.4690(13) . ?
O1 Y1 2.426(6) . ?
O2 Y1 2.263(6) . ?
O3 Y1 2.269(5) . ?
O4 Y1 2.421(6) . ?
O5 Y1 2.419(7) . ?
O6 Y1 2.412(6) . ?
O7 Y1 2.398(7) . ?
O8 Y1 2.357(6) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 124.9(8) . . ?
C3 C2 C7 122.5(8) . . ?
O1 C2 C7 112.6(8) . . ?
C4 C3 C2 118.7(9) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 121.0(10) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 120.7(10) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 119.6(9) . . ?
C5 C6 C8 116.9(9) . . ?
C7 C6 C8 123.5(8) . . ?
O2 C7 C2 117.4(7) . . ?
O2 C7 C6 125.1(8) . . ?
C2 C7 C6 117.5(8) . . ?
N1 C8 C6 128.2(9) . . ?
N1 C8 H8 115.9 . . ?
C6 C8 H8 115.9 . . ?
C10 C9 N1 115.6(9) . . ?
C10 C9 H9A 108.4 . . ?
N1 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
N1 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 116.9(11) . . ?
C9 C10 H10A 108.1 . . ?
C11 C10 H10A 108.1 . . ?
C9 C10 H10B 108.1 . . ?
C11 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
N2 C11 C10 112.6(10) . . ?
N2 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
N2 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N2 C12 C13 127.1(9) . . ?
N2 C12 H12 116.4 . . ?
C13 C12 H12 116.4 . . ?
C18 C13 C14 118.7(9) . . ?
C18 C13 C12 124.6(9) . . ?
C14 C13 C12 116.7(8) . . ?
C15 C14 C13 121.8(9) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C14 C15 C16 120.6(9) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 118.1(10) . . ?
C17 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
C16 C17 O4 124.1(9) . . ?
C16 C17 C18 122.4(9) . . ?
O4 C17 C18 113.5(8) . . ?
O3 C18 C13 124.7(8) . . ?
O3 C18 C17 116.8(8) . . ?
C13 C18 C17 118.5(8) . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 W1 178.7(8) . . ?
N4 C21 W1 178.5(9) . . ?
N10 C27 W1 176.3(9) . . ?
N5 C22 W1 179.1(8) . . ?
N6 C23 W1 177.8(9) . . ?
N7 C24 W1 174.4(9) . . ?
N8 C25 W1 178.3(10) . . ?
N9 C26 W1 173.8(11) . . ?
C8 N1 C9 115.7(8) . . ?
C8 N1 Ni1 122.2(6) . . ?
C9 N1 Ni1 121.4(7) . . ?
C12 N2 C11 118.8(8) . . ?
C12 N2 Ni1 124.7(6) . . ?
C11 N2 Ni1 116.3(7) . . ?
C20 N3 Ni1 163.0(7) . . ?
O3 Ni1 N2 91.9(3) . . ?
O3 Ni1 N1 168.7(3) . . ?
N2 Ni1 N1 98.9(3) . . ?
O3 Ni1 O2 77.0(2) . . ?
N2 Ni1 O2 168.8(3) . . ?
N1 Ni1 O2 92.2(3) . . ?
O3 Ni1 N3 95.4(3) . . ?
N2 Ni1 N3 91.8(3) . . ?
N1 Ni1 N3 87.7(3) . . ?
O2 Ni1 N3 89.7(3) . . ?
O3 Ni1 O9 86.7(2) . . ?
N2 Ni1 O9 89.1(3) . . ?
N1 Ni1 O9 90.1(3) . . ?
O2 Ni1 O9 89.8(2) . . ?
N3 Ni1 O9 177.7(3) . . ?
O3 Ni1 Y1 38.44(16) . . ?
N2 Ni1 Y1 130.3(2) . . ?
N1 Ni1 Y1 130.7(2) . . ?
O2 Ni1 Y1 38.54(16) . . ?
N3 Ni1 Y1 92.8(2) . . ?
O9 Ni1 Y1 88.18(15) . . ?
C2 O1 C1 115.7(8) . . ?
C2 O1 Y1 118.7(5) . . ?
C1 O1 Y1 125.5(7) . . ?
C7 O2 Ni1 121.3(5) . . ?
C7 O2 Y1 125.1(5) . . ?
Ni1 O2 Y1 107.2(3) . . ?
C18 O3 Ni1 125.0(5) . . ?
C18 O3 Y1 125.0(5) . . ?
Ni1 O3 Y1 108.1(2) . . ?
C17 O4 C19 115.7(8) . . ?
C17 O4 Y1 118.4(5) . . ?
C19 O4 Y1 123.6(6) . . ?
C24 W1 C20 144.7(3) . . ?
C24 W1 C23 76.8(4) . . ?
C20 W1 C23 126.2(3) . . ?
C24 W1 C22 90.1(3) . . ?
C20 W1 C22 75.5(3) . . ?
C23 W1 C22 71.9(3) . . ?
C24 W1 C26 99.6(4) . . ?
C20 W1 C26 77.4(4) . . ?
C23 W1 C26 142.9(4) . . ?
C22 W1 C26 145.1(3) . . ?
C24 W1 C27 71.3(4) . . ?
C20 W1 C27 74.1(3) . . ?
C23 W1 C27 135.4(3) . . ?
C22 W1 C27 77.7(3) . . ?
C26 W1 C27 73.9(3) . . ?
C24 W1 C25 74.9(3) . . ?
C20 W1 C25 133.4(3) . . ?
C23 W1 C25 73.3(4) . . ?
C22 W1 C25 144.4(3) . . ?
C26 W1 C25 70.3(4) . . ?
C27 W1 C25 124.8(4) . . ?
C24 W1 C21 144.8(3) . . ?
C20 W1 C21 70.3(3) . . ?
C23 W1 C21 74.6(4) . . ?
C22 W1 C21 100.0(3) . . ?
C26 W1 C21 91.2(4) . . ?
C27 W1 C21 143.7(4) . . ?
C25 W1 C21 77.6(3) . . ?
O2 Y1 O3 67.7(2) . . ?
O2 Y1 O8 77.4(2) . . ?
O3 Y1 O8 76.1(2) . . ?
O2 Y1 O7 123.8(3) . . ?
O3 Y1 O7 141.8(2) . . ?
O8 Y1 O7 72.3(2) . . ?
O2 Y1 O6 142.0(2) . . ?
O3 Y1 O6 125.4(2) . . ?
O8 Y1 O6 137.6(2) . . ?
O7 Y1 O6 70.8(2) . . ?
O2 Y1 O5 85.5(2) . . ?
O3 Y1 O5 73.6(2) . . ?
O8 Y1 O5 149.0(2) . . ?
O7 Y1 O5 138.0(2) . . ?
O6 Y1 O5 68.3(2) . . ?
O2 Y1 O4 132.3(2) . . ?
O3 Y1 O4 66.2(2) . . ?
O8 Y1 O4 80.7(2) . . ?
O7 Y1 O4 87.8(3) . . ?
O6 Y1 O4 77.8(2) . . ?
O5 Y1 O4 92.6(3) . . ?
O2 Y1 O1 65.5(2) . . ?
O3 Y1 O1 129.3(2) . . ?
O8 Y1 O1 110.7(2) . . ?
O7 Y1 O1 82.5(3) . . ?
O6 Y1 O1 84.4(2) . . ?
O5 Y1 O1 84.5(3) . . ?
O4 Y1 O1 161.8(2) . . ?
O2 Y1 Ni1 34.22(15) . . ?
O3 Y1 Ni1 33.49(14) . . ?
O8 Y1 Ni1 74.36(15) . . ?
O7 Y1 Ni1 144.33(17) . . ?
O6 Y1 Ni1 144.89(18) . . ?
O5 Y1 Ni1 77.00(16) . . ?
O4 Y1 Ni1 99.05(15) . . ?
O1 Y1 Ni1 97.80(15) . . ?
 
_refine_diff_density_max    2.373
_refine_diff_density_min   -2.289
_refine_diff_density_rms    0.162

_shelxl_version_number 2014-3



 
data_shelx
 
_audit_creation_method            SHELXL-2014
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C27 H32 Eu N10 Ni O10 W' 
_chemical_formula_weight          1051.14

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Eu'  'Eu'  -0.1578   3.6682
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni'  'Ni'   0.3393   1.1124
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    8.9747(3)
_cell_length_b                    13.9587(4)
_cell_length_c                    27.4653(9)
_cell_angle_alpha                 90
_cell_angle_beta                  93.266(3)
_cell_angle_gamma                 90
_cell_volume                      3435.13(19)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     63827 
_cell_measurement_theta_min       2.08 
_cell_measurement_theta_max       33.80 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             green 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     2.032          
_exptl_crystal_F_000              2036
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.4 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.08 
_exptl_absorpt_coefficient_mu     5.755
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.2503 
_exptl_absorpt_correction_T_max   0.4927 
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                       
_diffrn_measurement_device_type   'STOE-IPDS II' 
_diffrn_measurement_method        'omega scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             31923
_diffrn_reflns_av_unetI/netI      0.0374
_diffrn_reflns_av_R_equivalents   0.0542
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -36
_diffrn_reflns_limit_l_max        35
_diffrn_reflns_theta_min          2.082
_diffrn_reflns_theta_max          27.999
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.916
_diffrn_measured_fraction_theta_full  0.937
_diffrn_reflns_Laue_measured_fraction_max    0.916
_diffrn_reflns_Laue_measured_fraction_full   0.937
_diffrn_reflns_point_group_measured_fraction_max   0.916
_diffrn_reflns_point_group_measured_fraction_full  0.937
_reflns_number_total              7591
_reflns_number_gt                 6471
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'X-Area'
_computing_cell_refinement        'X-Area'
_computing_data_reduction         'X-Area'
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0302P)²+12.8800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00100(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          7591
_refine_ls_number_parameters      452
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0467
_refine_ls_R_factor_gt            0.0369
_refine_ls_wR_factor_ref          0.0792
_refine_ls_wR_factor_gt           0.0760
_refine_ls_goodness_of_fit_ref    1.057
_refine_ls_restrained_S_all       1.057
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.6566(9) 0.3398(7) 0.0240(3) 0.061(2) Uani 1 1 d . . . . .
H1A H 0.6093 0.2931 0.0026 0.092 Uiso 1 1 calc R U . . .
H1B H 0.6701 0.3983 0.0064 0.092 Uiso 1 1 calc R U . . .
H1C H 0.7520 0.3160 0.0362 0.092 Uiso 1 1 calc R U . . .
C2 C 0.6207(6) 0.4246(4) 0.0983(2) 0.0299(12) Uani 1 1 d . . . . .
C3 C 0.7433(7) 0.4811(5) 0.0922(2) 0.0422(16) Uani 1 1 d . . . . .
H3 H 0.7946 0.4778 0.0638 0.051 Uiso 1 1 calc R U . . .
C4 C 0.7890(8) 0.5434(5) 0.1297(3) 0.0482(17) Uani 1 1 d . . . . .
H4 H 0.8718 0.5824 0.1262 0.058 Uiso 1 1 calc R U . . .
C5 C 0.7137(7) 0.5481(5) 0.1715(3) 0.0463(17) Uani 1 1 d . . . . .
H5 H 0.7469 0.5895 0.1964 0.056 Uiso 1 1 calc R U . . .
C6 C 0.5876(7) 0.4914(4) 0.1776(2) 0.0304(12) Uani 1 1 d . . . . .
C7 C 0.5395(6) 0.4274(4) 0.14041(19) 0.0256(11) Uani 1 1 d . . . . .
C8 C 0.5140(7) 0.5036(4) 0.2232(2) 0.0344(13) Uani 1 1 d . . . . .
H8 H 0.5656 0.5396 0.2471 0.041 Uiso 1 1 calc R U . . .
C9 C 0.3390(9) 0.5038(6) 0.2815(2) 0.057(2) Uani 1 1 d . . . . .
H9A H 0.4163 0.4885 0.3064 0.068 Uiso 1 1 calc R U . . .
H9B H 0.3289 0.5729 0.2806 0.068 Uiso 1 1 calc R U . . .
C10 C 0.1987(10) 0.4632(6) 0.2962(3) 0.064(2) Uani 1 1 d . . . . .
H10A H 0.1776 0.4901 0.3276 0.077 Uiso 1 1 calc R U . . .
H10B H 0.2127 0.3948 0.3007 0.077 Uiso 1 1 calc R U . . .
C11 C 0.0608(9) 0.4784(6) 0.2613(3) 0.055(2) Uani 1 1 d . . . . .
H11A H -0.0289 0.4689 0.2788 0.065 Uiso 1 1 calc R U . . .
H11B H 0.0601 0.5438 0.2492 0.065 Uiso 1 1 calc R U . . .
C12 C -0.0596(7) 0.3655(5) 0.2092(2) 0.0347(14) Uani 1 1 d . . . . .
H12 H -0.1400 0.3777 0.2282 0.042 Uiso 1 1 calc R U . . .
C13 C -0.0838(6) 0.2952(5) 0.1702(2) 0.0320(12) Uani 1 1 d . . . . .
C14 C -0.2231(7) 0.2477(5) 0.1679(2) 0.0428(16) Uani 1 1 d . . . . .
H14 H -0.2928 0.2629 0.1905 0.051 Uiso 1 1 calc R U . . .
C15 C -0.2568(7) 0.1803(6) 0.1336(2) 0.0457(17) Uani 1 1 d . . . . .
H15 H -0.3493 0.1500 0.1328 0.055 Uiso 1 1 calc R U . . .
C16 C -0.1544(7) 0.1560(5) 0.0994(2) 0.0424(16) Uani 1 1 d . . . . .
H16 H -0.1777 0.1099 0.0757 0.051 Uiso 1 1 calc R U . . .
C17 C -0.0186(6) 0.2012(5) 0.10128(19) 0.0313(12) Uani 1 1 d . . . . .
C18 C 0.0196(6) 0.2720(4) 0.13617(18) 0.0253(11) Uani 1 1 d . . . . .
C19 C 0.0804(8) 0.0941(5) 0.0417(3) 0.0511(18) Uani 1 1 d . . . . .
H19A H 0.1624 0.0883 0.0209 0.077 Uiso 1 1 calc R U . . .
H19B H 0.0812 0.0410 0.0639 0.077 Uiso 1 1 calc R U . . .
H19C H -0.0118 0.0944 0.0222 0.077 Uiso 1 1 calc R U . . .
C20 C 0.2050(6) 0.6069(4) 0.13913(18) 0.0255(11) Uani 1 1 d . . . . .
C21 C 0.0806(6) 0.6744(4) 0.06238(19) 0.0290(12) Uani 1 1 d . . . . .
C22 C 0.0313(6) 0.7387(4) 0.17778(18) 0.0256(11) Uani 1 1 d . . . . .
C23 C -0.0153(7) 0.8352(4) 0.0996(2) 0.0329(13) Uani 1 1 d . . . . .
C24 C 0.2367(7) 0.9007(4) 0.1474(2) 0.0340(13) Uani 1 1 d . . . . .
C25 C 0.2343(7) 0.8409(4) 0.0576(2) 0.0348(13) Uani 1 1 d . . . . .
C26 C 0.4033(7) 0.7208(5) 0.0971(2) 0.0384(15) Uani 1 1 d . . . . .
C27 C 0.3358(6) 0.7486(4) 0.18642(19) 0.0286(12) Uani 1 1 d . . . . .
Eu1 Eu 0.32908(3) 0.27322(2) 0.07947(2) 0.02326(8) Uani 1 1 d . . . . .
N1 N 0.3891(6) 0.4714(4) 0.23411(16) 0.0315(11) Uani 1 1 d . . . . .
N2 N 0.0604(5) 0.4120(4) 0.22003(16) 0.0307(11) Uani 1 1 d . . . . .
N3 N 0.2128(6) 0.5276(4) 0.14833(16) 0.0314(11) Uani 1 1 d . . . . .
N4 N 0.0199(6) 0.6307(4) 0.03181(18) 0.0410(13) Uani 1 1 d . . . . .
N5 N -0.0516(6) 0.7279(4) 0.20751(18) 0.0375(12) Uani 1 1 d . . . . .
N6 N -0.1220(7) 0.8752(5) 0.0872(2) 0.0544(16) Uani 1 1 d . . . . .
N7 N 0.2653(8) 0.9765(4) 0.1588(2) 0.0549(16) Uani 1 1 d . . . . .
N8 N 0.2661(8) 0.8850(5) 0.0246(2) 0.0561(17) Uani 1 1 d . . . . .
N9 N 0.5173(7) 0.7066(6) 0.0825(2) 0.068(2) Uani 1 1 d . . . . .
N10 N 0.4197(6) 0.7452(4) 0.2191(2) 0.0455(14) Uani 1 1 d . . . . .
Ni1 Ni 0.25149(8) 0.39811(5) 0.18582(2) 0.02325(15) Uani 1 1 d . . . . .
O1 O 0.5639(4) 0.3577(3) 0.06439(14) 0.0358(10) Uani 1 1 d . . . . .
O2 O 0.4230(4) 0.3684(3) 0.14261(12) 0.0257(8) Uani 1 1 d . . . . .
O3 O 0.1513(4) 0.3147(3) 0.13369(12) 0.0253(8) Uani 1 1 d . . . . .
O4 O 0.0944(5) 0.1826(3) 0.06897(14) 0.0341(9) Uani 1 1 d . . . . .
O5 O 0.2059(6) 0.4210(3) 0.04760(16) 0.0475(12) Uani 1 1 d . . . . .
O6 O 0.2890(5) 0.2688(4) -0.00980(14) 0.0423(11) Uani 1 1 d . . . . .
O7 O 0.4570(6) 0.1329(4) 0.04740(16) 0.0500(12) Uani 1 1 d . . . . .
O8 O 0.3654(5) 0.1605(3) 0.14556(13) 0.0320(9) Uani 1 1 d . . . . .
O9 O 0.2986(4) 0.2624(3) 0.22774(13) 0.0283(8) Uani 1 1 d . . . . .
O10 O 0.5853(8) 0.9581(6) 0.0708(5) 0.167(5) Uani 1 1 d . . . . .
W1 W 0.18731(2) 0.75761(2) 0.12135(2) 0.02060(7) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.445(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.371(8) . ?
C2 O1 1.395(7) . ?
C2 C7 1.403(7) . ?
C3 C4 1.392(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.406(7) . ?
C6 C8 1.459(8) . ?
C7 O2 1.335(6) . ?
C7 Eu1 3.262(5) . ?
C8 N1 1.259(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.458(11) . ?
C9 N1 1.473(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.537(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.464(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N2 1.278(8) . ?
C12 C13 1.459(9) . ?
C12 H12 0.9300 . ?
C13 C18 1.393(8) . ?
C13 C14 1.414(8) . ?
C14 C15 1.354(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.393(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.371(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.405(8) . ?
C17 O4 1.409(7) . ?
C18 O3 1.329(6) . ?
C18 Eu1 3.261(5) . ?
C19 O4 1.446(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N3 1.137(7) . ?
C20 W1 2.163(6) . ?
C21 N4 1.150(7) . ?
C21 W1 2.171(5) . ?
C22 N5 1.146(7) . ?
C22 W1 2.163(5) . ?
C23 N6 1.144(8) . ?
C23 W1 2.171(6) . ?
C24 N7 1.129(8) . ?
C24 W1 2.159(6) . ?
C25 N8 1.146(8) . ?
C25 W1 2.162(6) . ?
C26 N9 1.138(8) . ?
C26 W1 2.148(6) . ?
C27 N10 1.140(7) . ?
C27 W1 2.171(5) . ?
Eu1 O2 2.306(3) . ?
Eu1 O3 2.317(3) . ?
Eu1 O8 2.410(4) . ?
Eu1 O6 2.459(4) . ?
Eu1 O7 2.459(4) . ?
Eu1 O4 2.460(4) . ?
Eu1 O1 2.470(4) . ?
Eu1 O5 2.476(4) . ?
Eu1 Ni1 3.5054(7) . ?
N1 Ni1 2.036(5) . ?
N2 Ni1 2.011(5) . ?
N3 Ni1 2.100(5) . ?
Ni1 O3 2.017(4) . ?
Ni1 O2 2.039(4) . ?
Ni1 O9 2.244(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 124.7(5) . . ?
C3 C2 C7 122.9(6) . . ?
O1 C2 C7 112.4(5) . . ?
C2 C3 C4 118.3(6) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 120.8(6) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 121.0(6) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C7 119.4(5) . . ?
C5 C6 C8 116.4(5) . . ?
C7 C6 C8 124.2(5) . . ?
O2 C7 C2 117.7(5) . . ?
O2 C7 C6 124.6(5) . . ?
C2 C7 C6 117.7(5) . . ?
O2 C7 Eu1 35.3(2) . . ?
C2 C7 Eu1 82.6(3) . . ?
C6 C7 Eu1 159.5(4) . . ?
N1 C8 C6 128.0(5) . . ?
N1 C8 H8 116.0 . . ?
C6 C8 H8 116.0 . . ?
C10 C9 N1 115.9(6) . . ?
C10 C9 H9A 108.3 . . ?
N1 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
N1 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 116.8(7) . . ?
C9 C10 H10A 108.1 . . ?
C11 C10 H10A 108.1 . . ?
C9 C10 H10B 108.1 . . ?
C11 C10 H10B 108.1 . . ?
H10A C10 H10B 107.3 . . ?
N2 C11 C10 111.1(6) . . ?
N2 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
N2 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N2 C12 C13 126.9(5) . . ?
N2 C12 H12 116.6 . . ?
C13 C12 H12 116.6 . . ?
C18 C13 C14 118.8(6) . . ?
C18 C13 C12 124.9(5) . . ?
C14 C13 C12 116.3(5) . . ?
C15 C14 C13 121.3(6) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 120.6(6) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 118.7(6) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C16 C17 C18 122.1(6) . . ?
C16 C17 O4 124.1(5) . . ?
C18 C17 O4 113.8(5) . . ?
O3 C18 C13 123.9(5) . . ?
O3 C18 C17 117.6(5) . . ?
C13 C18 C17 118.4(5) . . ?
O3 C18 Eu1 35.8(2) . . ?
C13 C18 Eu1 159.6(4) . . ?
C17 C18 Eu1 81.9(3) . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 W1 179.3(5) . . ?
N4 C21 W1 177.9(5) . . ?
N5 C22 W1 179.4(5) . . ?
N6 C23 W1 178.5(6) . . ?
N7 C24 W1 176.5(6) . . ?
N8 C25 W1 176.8(6) . . ?
N9 C26 W1 175.5(7) . . ?
N10 C27 W1 176.5(5) . . ?
O2 Eu1 O3 66.96(12) . . ?
O2 Eu1 O8 77.39(13) . . ?
O3 Eu1 O8 75.37(13) . . ?
O2 Eu1 O6 142.26(14) . . ?
O3 Eu1 O6 125.46(14) . . ?
O8 Eu1 O6 137.80(15) . . ?
O2 Eu1 O7 124.76(15) . . ?
O3 Eu1 O7 141.42(15) . . ?
O8 Eu1 O7 72.78(14) . . ?
O6 Eu1 O7 70.60(16) . . ?
O2 Eu1 O4 131.19(13) . . ?
O3 Eu1 O4 65.63(13) . . ?
O8 Eu1 O4 80.25(14) . . ?
O6 Eu1 O4 78.15(14) . . ?
O7 Eu1 O4 87.85(16) . . ?
O2 Eu1 O1 64.67(12) . . ?
O3 Eu1 O1 127.88(13) . . ?
O8 Eu1 O1 110.95(14) . . ?
O6 Eu1 O1 85.56(14) . . ?
O7 Eu1 O1 84.24(16) . . ?
O4 Eu1 O1 163.49(12) . . ?
O2 Eu1 O5 85.56(14) . . ?
O3 Eu1 O5 73.10(14) . . ?
O8 Eu1 O5 148.03(14) . . ?
O6 Eu1 O5 68.36(15) . . ?
O7 Eu1 O5 138.17(15) . . ?
O4 Eu1 O5 91.44(16) . . ?
O1 Eu1 O5 84.91(16) . . ?
O2 Eu1 C18 85.92(13) . . ?
O3 Eu1 C18 19.60(13) . . ?
O8 Eu1 C18 73.68(13) . . ?
O6 Eu1 C18 113.32(13) . . ?
O7 Eu1 C18 126.48(16) . . ?
O4 Eu1 C18 46.07(13) . . ?
O1 Eu1 C18 147.22(14) . . ?
O5 Eu1 C18 78.35(15) . . ?
O2 Eu1 C7 19.55(12) . . ?
O3 Eu1 C7 84.56(13) . . ?
O8 Eu1 C7 89.70(13) . . ?
O6 Eu1 C7 125.15(14) . . ?
O7 Eu1 C7 116.17(16) . . ?
O4 Eu1 C7 150.03(13) . . ?
O1 Eu1 C7 45.31(13) . . ?
O5 Eu1 C7 82.26(15) . . ?
C18 Eu1 C7 104.03(13) . . ?
O2 Eu1 Ni1 33.72(9) . . ?
O3 Eu1 Ni1 33.24(9) . . ?
O8 Eu1 Ni1 73.84(9) . . ?
O6 Eu1 Ni1 144.95(11) . . ?
O7 Eu1 Ni1 144.45(11) . . ?
O4 Eu1 Ni1 98.28(9) . . ?
O1 Eu1 Ni1 96.56(9) . . ?
O5 Eu1 Ni1 76.96(10) . . ?
C18 Eu1 Ni1 52.39(10) . . ?
C7 Eu1 Ni1 51.75(9) . . ?
C8 N1 C9 115.0(5) . . ?
C8 N1 Ni1 122.6(4) . . ?
C9 N1 Ni1 121.7(4) . . ?
C12 N2 C11 117.8(5) . . ?
C12 N2 Ni1 124.9(4) . . ?
C11 N2 Ni1 117.3(4) . . ?
C20 N3 Ni1 162.5(4) . . ?
N2 Ni1 O3 91.70(17) . . ?
N2 Ni1 N1 98.6(2) . . ?
O3 Ni1 N1 169.11(18) . . ?
N2 Ni1 O2 169.60(18) . . ?
O3 Ni1 O2 77.90(14) . . ?
N1 Ni1 O2 91.78(17) . . ?
N2 Ni1 N3 91.41(19) . . ?
O3 Ni1 N3 95.43(17) . . ?
N1 Ni1 N3 87.95(19) . . ?
O2 Ni1 N3 89.94(17) . . ?
N2 Ni1 O9 88.97(17) . . ?
O3 Ni1 O9 86.56(15) . . ?
N1 Ni1 O9 90.02(17) . . ?
O2 Ni1 O9 90.04(15) . . ?
N3 Ni1 O9 177.96(17) . . ?
N2 Ni1 Eu1 130.72(14) . . ?
O3 Ni1 Eu1 39.02(10) . . ?
N1 Ni1 Eu1 130.60(14) . . ?
O2 Ni1 Eu1 38.88(10) . . ?
N3 Ni1 Eu1 93.14(12) . . ?
O9 Ni1 Eu1 88.12(10) . . ?
C2 O1 C1 115.1(5) . . ?
C2 O1 Eu1 119.4(3) . . ?
C1 O1 Eu1 125.4(4) . . ?
C7 O2 Ni1 121.3(3) . . ?
C7 O2 Eu1 125.1(3) . . ?
Ni1 O2 Eu1 107.39(16) . . ?
C18 O3 Ni1 125.8(3) . . ?
C18 O3 Eu1 124.6(3) . . ?
Ni1 O3 Eu1 107.74(15) . . ?
C17 O4 C19 116.1(5) . . ?
C17 O4 Eu1 118.2(3) . . ?
C19 O4 Eu1 123.3(4) . . ?
C26 W1 C24 98.8(3) . . ?
C26 W1 C25 69.9(2) . . ?
C24 W1 C25 74.1(2) . . ?
C26 W1 C20 77.4(2) . . ?
C24 W1 C20 144.4(2) . . ?
C25 W1 C20 133.7(2) . . ?
C26 W1 C22 145.6(2) . . ?
C24 W1 C22 90.3(2) . . ?
C25 W1 C22 144.1(2) . . ?
C20 W1 C22 76.2(2) . . ?
C26 W1 C21 90.5(2) . . ?
C24 W1 C21 144.7(2) . . ?
C25 W1 C21 77.4(2) . . ?
C20 W1 C21 70.8(2) . . ?
C22 W1 C21 101.1(2) . . ?
C26 W1 C23 142.3(2) . . ?
C24 W1 C23 77.5(2) . . ?
C25 W1 C23 73.1(2) . . ?
C20 W1 C23 126.6(2) . . ?
C22 W1 C23 72.0(2) . . ?
C21 W1 C23 74.6(2) . . ?
C26 W1 C27 73.7(2) . . ?
C24 W1 C27 71.1(2) . . ?
C25 W1 C27 123.9(2) . . ?
C20 W1 C27 74.0(2) . . ?
C22 W1 C27 78.2(2) . . ?
C21 W1 C27 143.8(2) . . ?
C23 W1 C27 136.1(2) . . ?
 
_refine_diff_density_max    1.068
_refine_diff_density_min   -0.985
_refine_diff_density_rms    0.143

_shelxl_version_number 2014-3



data_global 
_audit_creation_date        "2016-04-05"
_audit_creation_method CRYSTALS_ver_14.61

_oxford_structure_analysis_title  'THIS IS THE DEFAULT SETTING FOR THE TITLE, P'
_chemical_name_systematic         ?
_chemical_melting_point           ?

#looking for refcif 
 
 
# Check this file using the IUCr facility at: 
# http://checkcif.iucr.org/ 
 
# The content below is held in the file 'script/refcif.dat'. This is a text 
# file which you may edit to reflect local conditions. 
# Items which need looking at are represented by a '?'. 
# Items for which there are choices are prefixed with 'choose from'. 
 
_publ_contact_letter 
; 
; 
_publ_contact_author_name         '' 
_publ_contact_author_address 
; 
; 
 
_publ_contact_author_phone        '' 
_publ_contact_author_fax          '' 
_publ_contact_author_email        '' 
_publ_requested_journal           '' 
_publ_requested_category          EO # choose from: FI FM FO CI CM CO AD 
_publ_requested_coeditor_name     '' 
 
_publ_section_title 
# Title of paper - generally just the systematic or trivial name 
; ? 
; 
 
# The loop structure below should contain the names and addresses of all 
# authors, in the required order of publication. Repeat as necessary. 
loop_ 
 _publ_author_name 
 _publ_author_address 
 _publ_author_footnote 
 'Other, Anthony N.' # Author 1 
; 
 ? # Address for author 1 
; 
; 
 ? # Footnote for author 1 
; 
 'Else, S. O.' # Author 2 
; 
 ? # Address 2 
; 
; 
 ? # Footnote 2 
; 
 
 
_publ_section_abstract 
# Text of the abstract 
# (a) The Abstract must be self-contained and comprehensible 
# without the rest of the paper. This means no references 
# to atom names or to compound numbers; compounds must be 
# identified as the title compound, or by name or by some other 
# means such as derivatives of each other (e.g. "the 
# corresponding ketone"). 
# (b) The chemical formula of "the title compound" must be given. 
# (c) Any crystallographic molecular symmetry should be 
# mentioned, and also the presence of more than one molecule 
# in the asymmetric unit (i.e. anything other than Z'=1). 
; 
? 
; 
 
_publ_section_related_literature  # Not in version 2.3.1 
############################################################### 
# Essential references (e.g. to the origin of the material studied, related 
# structural studies, and to information supporting the reported structure) 
# should be cited in this section, with appropriate very brief explanatory 
# text, for example `The synthesis of the complex is described by Jones 
# (2001). The anhydrous complex has essentially the same coordination 
# geometry (Smith, 2003).' In addition, all references included in the 
# supplementary materials, but not elsewhere in the published article, 
# should be given here. The simple text `For related literature, see:...' 
# may be used, but further details should be provided in the Comment 
# section, which forms part of the supplementary material. 
############################################################### 
; 
? 
; 
 
_publ_section_comment 
# Text of the paper 
# Note that atoms are referenced as N2, not N(2) or N~2~ 
# If text containing () occur within (), the outer ones should be [] 
# Figures should be referenced as Fig. 
; 
? 
; 
_publ_section_acknowledgements    # Acknowledgments 
; 
? 
; 
_publ_section_figure_captions 
# Captions to figures - Start each caption on a new line after a blank line 
; 
; 
 
 
_publ_section_exptl_refinement 
# Some potentially useful phrases are donated by Bill Clegg: 
; 

The H atoms were refined with riding constraints 
(Cooper et al, 2010). 
 
Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 
43, 1100-1107. 

Hydrogen atoms could not be located on the 6 H2O molecules
 
; 
 
_publ_section_exptl_prep 
# Brief details or a reference. Include solvent if known 
; 
? 
; 
 
# Hand-made tables can be put in the cif. The number of columns 
# is set in the loop header. 
# The contants of each column can either be a piece of text 
# without any spaces (eg a number) or other text enclosed in " " 
# Remove the leading # in the following example 
 
#geom_extra_table_head_A 
#; 
#Table 2. 
#Molecular parameters deviating most from MOGUL averages 
#; 
# 
#loop_ 
#_geom_extra_tableA_col_1 
#_geom_extra_tableA_col_2 
#_geom_extra_tableA_col_3 
#_geom_extra_tableA_col_4 
# 
#Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" 
#N5-C6-C4 129 124 "7 (\%)" 
#C3-O10-C2 105 109 "2 (\%)" 
#C6-O7 1.25 1.22 ".02 (\%A)" 
# 
 
data_1 
 
_exptl_special_details 
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
; 
_refine_special_details 
; 
? 
; 
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 
 
# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 
 
# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 
 
# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 
 
# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 
 
# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                    8.9103(3)
_cell_length_b                    13.9215(5)
_cell_length_c                    27.2730(10)
_cell_angle_alpha                 90
_cell_angle_beta                  93.553(4)
_cell_angle_gamma                 90
_cell_volume                      3376.6(2)
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M    'P 1 21/c 1 ' 
_symmetry_space_group_name_Hall   '-P 2ybc ' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,-y,-z'
 '-x,y+1/2,-z+1/2'
 'x,-y+1/2,z+1/2'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0061   0.0033  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 P       0.1023   0.0942   6.4345   1.9067   4.1791  27.1570   1.7800   0.5260
   1.4908  68.1645   1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Ni      0.3393   1.1124  12.8376   3.8785   7.2920   0.2565   4.4438  12.1763
   2.3800  66.3421   1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Gd     -0.1653   3.9035  25.0709   2.2534  19.0798   0.1820  13.8518  12.9331
   3.5454 101.3980   2.4196 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 W      -0.8490   6.8722  29.0818   1.7203  15.4300   9.2259  14.4327   0.3217
   5.1198  57.0560   9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    4

# Given Formula = C27 H32 Gd1 N10 Ni1 O10 W1 
# Dc =      2.08 Fooo =   1992.00 Mu =     59.61 M =   1056.42
# Found Formula = C27 H20 Gd1 N10 Ni1 O10 W1 
# Dc =      2.05 FOOO =   1992.00 Mu =     59.60 M =   1044.33

_chemical_formula_sum             'C27 H32 Gd1 N10 Ni1 O10 W1'
_chemical_formula_moiety          'C27 H30 Gd1 N10 Ni1 O9 W1, H2 O'
_chemical_compound_source                ?
_chemical_formula_weight           1056.42
 
 
_cell_measurement_reflns_used        13133
_cell_measurement_theta_min              2
_cell_measurement_theta_max             29
_cell_measurement_temperature          180
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'green' 
_exptl_crystal_size_min           0.120 
_exptl_crystal_size_mid           0.150 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     2.078 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              1992 
_exptl_absorpt_coefficient_mu     5.961 
 
# Sheldrick geometric approximatio 0.41 0.49 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'CrysAlisPro, (Agilent, 2011)' 
_exptl_absorpt_correction_T_min   0.36 
_exptl_absorpt_correction_T_max   0.52 
_diffrn_measurement_device_type   'Oxford Diffraction XCALIBUR' 
_diffrn_measurement_device        'Area' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71070
_diffrn_measurement_method        'φ & ω scans' 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'Xcalibur, (Oxford Diffraction, 2002)' 
_computing_cell_refinement        'CrysAlisPro, (Agilent, 2011)' 
_computing_data_reduction         'XRED (Stoe & Cie 1996)' 
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        180
_diffrn_reflns_number             31324 
_reflns_number_total              8942 
_diffrn_reflns_av_R_equivalents   0.080 
# Number of reflections without Friedels Law is 8942 
# Number of reflections with Friedels Law is 0 
# Theoretical number of reflections is about 9117 
 
 
_diffrn_reflns_theta_min          2.679 
_diffrn_reflns_theta_max          29.219 
_diffrn_measured_fraction_theta_max 0.988 
 
_diffrn_reflns_theta_full         28.635 
_diffrn_measured_fraction_theta_full 0.996 
 
 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -37 
_diffrn_reflns_limit_l_max        37 
_reflns_limit_h_min               -12 
_reflns_limit_h_max               12 
_reflns_limit_k_min               0 
_reflns_limit_k_max               19 
_reflns_limit_l_min               0 
_reflns_limit_l_max               37 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -2.89 
_refine_diff_density_max          4.00 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>1.7\s(I)
_refine_ls_number_reflns          4623 
_refine_ls_number_restraints      0 
_refine_ls_number_parameters      460 
_oxford_refine_ls_R_factor_ref    0.0449 
_refine_ls_wR_factor_ref          0.0545 
_refine_ls_goodness_of_fit_ref    0.9978 
_refine_ls_shift/su_max           0.0005720 
_refine_ls_shift/su_mean          0.0000271 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         9054 
_refine_ls_R_factor_all           0.0936 
_refine_ls_wR_factor_all          0.1360 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 4341 
_refine_ls_R_factor_gt            0.0435 
_refine_ls_wR_factor_gt           0.0532 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  '.' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     constr         #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
 
# WARNING. The IUCr will not accept pure Unit Weights for F-squared refinements 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./4Fsq 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Agilent (2011). CrysAlisPro. 
 
Oxford Diffraction, (2002). Xcalibur User Manual. 
 
Stoe & Cie (1996). IPDS Software. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
W1 W 0.18710(6) 0.74315(4) 0.121097(17) 0.0151 1.0000 Uani . . . . . . 
Gd1 Gd 0.32921(7) 1.22830(4) 0.07970(2) 0.0166 1.0000 Uani . . . . . . 
Ni1 Ni 0.2516(2) 1.10273(11) 0.18592(6) 0.0172 1.0000 Uani . . . . . . 
C1 C 0.2049(16) 0.8929(10) 0.1391(5) 0.0236 1.0000 Uani . . . . . . 
C2 C 0.4039(15) 0.7825(12) 0.0965(4) 0.0278 1.0000 Uani . . . . . . 
C3 C 0.3361(15) 0.7528(10) 0.1864(5) 0.0252 1.0000 Uani . . . . . . 
C4 C 0.2336(18) 0.6008(10) 0.1476(5) 0.0271 1.0000 Uani . . . . . . 
C5 C 0.2341(19) 0.6582(11) 0.0577(5) 0.0320 1.0000 Uani . . . . . . 
C6 C -0.0185(19) 0.6665(10) 0.0990(5) 0.0289 1.0000 Uani . . . . . . 
C7 C 0.0291(14) 0.7632(9) 0.1784(4) 0.0221 1.0000 Uani . . . . . . 
C8 C 0.0823(15) 0.8270(9) 0.0614(5) 0.0206 1.0000 Uani . . . . . . 
C9 C 0.082(2) 1.4080(12) 0.0417(6) 0.0390 1.0000 Uani . . . . . . 
C10 C -0.0206(17) 1.3013(11) 0.1015(5) 0.0259 1.0000 Uani . . . . . . 
C11 C -0.1556(17) 1.3473(12) 0.0994(6) 0.0325 1.0000 Uani . . . . . . 
C12 C -0.2602(16) 1.3230(12) 0.1335(6) 0.0328 1.0000 Uani . . . . . . 
C13 C -0.2227(15) 1.2532(13) 0.1682(5) 0.0339 1.0000 Uani . . . . . . 
C14 C -0.0882(16) 1.2055(11) 0.1705(5) 0.0264 1.0000 Uani . . . . . . 
C15 C 0.0185(13) 1.2290(9) 0.1351(5) 0.0205 1.0000 Uani . . . . . . 
C16 C -0.0612(16) 1.1352(10) 0.2087(5) 0.0260 1.0000 Uani . . . . . . 
C17 C 0.062(2) 1.0201(11) 0.2614(6) 0.0376 1.0000 Uani . . . . . . 
C18 C 0.194(2) 1.0382(13) 0.2960(6) 0.0430 1.0000 Uani . . . . . . 
C19 C 0.339(2) 0.9954(12) 0.2816(6) 0.0425 1.0000 Uani . . . . . . 
C20 C 0.5157(17) 0.9961(10) 0.2235(5) 0.0262 1.0000 Uani . . . . . . 
C21 C 0.5901(16) 1.0089(9) 0.1772(5) 0.0212 1.0000 Uani . . . . . . 
C22 C 0.5416(13) 1.0734(9) 0.1408(5) 0.0173 1.0000 Uani . . . . . . 
C23 C 0.7149(18) 0.9532(11) 0.1708(6) 0.0320 1.0000 Uani . . . . . . 
C24 C 0.7904(18) 0.9567(12) 0.1287(6) 0.0375 1.0000 Uani . . . . . . 
C25 C 0.7468(16) 1.0204(11) 0.0920(6) 0.0286 1.0000 Uani . . . . . . 
C26 C 0.6239(15) 1.0777(9) 0.0979(5) 0.0217 1.0000 Uani . . . . . . 
C27 C 0.6583(17) 1.1648(13) 0.0251(5) 0.0351 1.0000 Uani . . . . . . 
N1 N 0.2116(14) 0.9734(7) 0.1475(4) 0.0239 1.0000 Uani . . . . . . 
N2 N 0.5193(16) 0.7977(14) 0.0824(5) 0.0552 1.0000 Uani . . . . . . 
N3 N 0.4219(14) 0.7560(11) 0.2197(4) 0.0357 1.0000 Uani . . . . . . 
N4 N 0.2619(18) 0.5242(9) 0.1581(5) 0.0378 1.0000 Uani . . . . . . 
N5 N 0.2635(19) 0.6124(10) 0.0243(5) 0.0457 1.0000 Uani . . . . . . 
N6 N -0.1239(16) 0.6267(10) 0.0866(5) 0.0372 1.0000 Uani . . . . . . 
N7 N -0.0514(14) 0.7735(9) 0.2077(4) 0.0281 1.0000 Uani . . . . . . 
N8 N 0.0182(14) 0.8700(10) 0.0312(4) 0.0293 1.0000 Uani . . . . . . 
N9 N 0.0584(14) 1.0877(8) 0.2198(4) 0.0227 1.0000 Uani . . . . . . 
N10 N 0.3886(14) 1.0293(8) 0.2340(4) 0.0235 1.0000 Uani . . . . . . 
O1 O 0.0947(12) 1.3188(7) 0.0692(3) 0.0271 1.0000 Uani . . . . . . 
O2 O 0.1507(11) 1.1855(6) 0.1334(3) 0.0219 1.0000 Uani . . . . . . 
O3 O 0.4247(10) 1.1328(6) 0.1432(3) 0.0179 1.0000 Uani . . . . . . 
O4 O 0.5635(11) 1.1453(7) 0.0647(3) 0.0251 1.0000 Uani . . . . . . 
O5 O 0.2114(13) 1.0807(7) 0.0478(4) 0.0351 1.0000 Uani . . . . . . 
O6 O 0.2901(11) 1.2334(8) -0.0097(3) 0.0305 1.0000 Uani . . . . . . 
O7 O 0.4573(14) 1.3690(8) 0.0481(4) 0.0396 1.0000 Uani . . . . . . 
O8 O 0.3663(11) 1.3397(7) 0.1458(3) 0.0217 1.0000 Uani . . . . . . 
O9 O 0.2978(10) 1.2376(7) 0.2273(3) 0.0204 1.0000 Uani . . . . . . 
O10 O 0.581(3) 0.5308(19) 0.0873(12) 0.0532 0.5000 Uani . . . . . . 
O11 O 0.590(3) 0.5530(18) 0.0545(10) 0.0478 0.5000 Uani . . . . . . 
H93 H 0.1643 1.4132 0.0210 0.0620 1.0000 Uiso R . . . . . 
H92 H 0.0833 1.4618 0.0637 0.0620 1.0000 Uiso R . . . . . 
H91 H -0.0110 1.4078 0.0219 0.0620 1.0000 Uiso R . . . . . 
H111 H -0.1773 1.3945 0.0759 0.0390 1.0000 Uiso R . . . . . 
H121 H -0.3533 1.3533 0.1327 0.0400 1.0000 Uiso R . . . . . 
H131 H -0.2920 1.2375 0.1910 0.0410 1.0000 Uiso R . . . . . 
H161 H -0.1412 1.1228 0.2279 0.0320 1.0000 Uiso R . . . . . 
H171 H -0.0295 1.0267 0.2783 0.0460 1.0000 Uiso R . . . . . 
H172 H 0.0701 0.9551 0.2490 0.0460 1.0000 Uiso R . . . . . 
H181 H 0.2075 1.1072 0.2985 0.0540 1.0000 Uiso R . . . . . 
H182 H 0.1725 1.0122 0.3277 0.0540 1.0000 Uiso R . . . . . 
H191 H 0.4180 1.0105 0.3066 0.0510 1.0000 Uiso R . . . . . 
H192 H 0.3255 0.9265 0.2798 0.0510 1.0000 Uiso R . . . . . 
H201 H 0.5668 0.9590 0.2477 0.0310 1.0000 Uiso R . . . . . 
H231 H 0.7487 0.9120 0.1958 0.0380 1.0000 Uiso R . . . . . 
H241 H 0.8714 0.9160 0.1249 0.0430 1.0000 Uiso R . . . . . 
H251 H 0.7991 1.0246 0.0636 0.0341 1.0000 Uiso R . . . . . 
H273 H 0.6161 1.2171 0.0061 0.0530 1.0000 Uiso R . . . . . 
H272 H 0.7575 1.1816 0.0382 0.0529 1.0000 Uiso R . . . . . 
H271 H 0.6628 1.1085 0.0049 0.0530 1.0000 Uiso R . . . . . 

_refine_ls_extinction_method 
    'None'
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
W1 . C1 . 2.145(15)    yes
W1 . C2 . 2.154(13)    yes
W1 . C3 . 2.159(14)    yes
W1 . C4 . 2.140(15)    yes
W1 . C5 . 2.156(14)    yes
W1 . C6 . 2.173(16)    yes
W1 . C7 . 2.185(12)    yes
W1 . C8 . 2.167(14)    yes
Gd1 . O1 . 2.442(10)    yes
Gd1 . O2 . 2.307(9)    yes
Gd1 . O3 . 2.305(8)    yes
Gd1 . O4 . 2.442(9)    yes
Gd1 . O5 . 2.444(10)    yes
Gd1 . O6 . 2.442(9)    yes
Gd1 . O7 . 2.450(10)    yes
Gd1 . O8 . 2.386(9)    yes
Ni1 . N1 . 2.102(11)    yes
Ni1 . N9 . 2.015(11)    yes
Ni1 . N10 . 2.015(12)    yes
Ni1 . O2 . 2.006(10)    yes
Ni1 . O3 . 2.033(9)    yes
Ni1 . O9 . 2.216(9)    yes
C1 . N1 . 1.144(18)    yes
C2 . N2 . 1.140(18)    yes
C3 . N3 . 1.149(17)    yes
C4 . N4 . 1.129(19)    yes
C5 . N5 . 1.157(19)    yes
C6 . N6 . 1.125(19)    yes
C7 . N7 . 1.117(16)    yes
C8 . N8 . 1.143(17)    yes
C9 . O1 . 1.452(18)    yes
C9 . H93 . 0.956    no
C9 . H92 . 0.960    no
C9 . H91 . 0.959    no
C10 . C11 . 1.36(2)    yes
C10 . C15 . 1.392(19)    yes
C10 . O1 . 1.414(17)    yes
C11 . C12 . 1.40(2)    yes
C11 . H111 . 0.931    no
C12 . C13 . 1.38(2)    yes
C12 . H121 . 0.929    no
C13 . C14 . 1.37(2)    yes
C13 . H131 . 0.927    no
C14 . C15 . 1.432(17)    yes
C14 . C16 . 1.44(2)    yes
C15 . O2 . 1.328(14)    yes
C16 . N9 . 1.274(18)    yes
C16 . H161 . 0.926    no
C17 . C18 . 1.48(2)    yes
C17 . N9 . 1.472(18)    yes
C17 . H171 . 0.967    no
C17 . H172 . 0.969    no
C18 . C19 . 1.50(2)    yes
C18 . H181 . 0.969    no
C18 . H182 . 0.969    no
C19 . N10 . 1.473(17)    yes
C19 . H191 . 0.971    no
C19 . H192 . 0.969    no
C20 . C21 . 1.474(18)    yes
C20 . N10 . 1.272(18)    yes
C20 . H201 . 0.932    no
C21 . C22 . 1.387(17)    yes
C21 . C23 . 1.375(19)    yes
C22 . C26 . 1.420(17)    yes
C22 . O3 . 1.334(14)    yes
C23 . C24 . 1.37(2)    yes
C23 . H231 . 0.927    no
C24 . C25 . 1.38(2)    yes
C24 . H241 . 0.929    no
C25 . C26 . 1.373(18)    yes
C25 . H251 . 0.930    no
C26 . O4 . 1.391(16)    yes
C27 . O4 . 1.437(15)    yes
C27 . H273 . 0.957    no
C27 . H272 . 0.961    no
C27 . H271 . 0.961    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
C1 . W1 . C2 . 76.7(5)    yes
C1 . W1 . C3 . 73.6(5)    yes
C2 . W1 . C3 . 74.0(4)    yes
C1 . W1 . C4 . 144.3(5)    yes
C2 . W1 . C4 . 100.5(6)    yes
C3 . W1 . C4 . 71.5(6)    yes
C1 . W1 . C5 . 134.5(5)    yes
C2 . W1 . C5 . 70.6(6)    yes
C3 . W1 . C5 . 123.7(6)    yes
C4 . W1 . C5 . 73.7(5)    yes
C1 . W1 . C6 . 126.1(6)    yes
C2 . W1 . C6 . 142.7(5)    yes
C3 . W1 . C6 . 136.4(5)    yes
C4 . W1 . C6 . 77.4(6)    yes
C5 . W1 . C6 . 73.2(6)    yes
C1 . W1 . C7 . 75.7(5)    yes
C2 . W1 . C7 . 145.1(5)    yes
C3 . W1 . C7 . 78.0(5)    yes
C4 . W1 . C7 . 89.9(5)    yes
C5 . W1 . C7 . 144.0(5)    yes
C1 . W1 . C8 . 70.8(5)    yes
C2 . W1 . C8 . 89.0(5)    yes
C3 . W1 . C8 . 143.2(5)    yes
C4 . W1 . C8 . 144.8(5)    yes
C5 . W1 . C8 . 77.8(5)    yes
C6 . W1 . C7 . 72.0(5)    yes
C6 . W1 . C8 . 74.9(5)    yes
C7 . W1 . C8 . 101.6(5)    yes
O1 . Gd1 . O2 . 65.7(3)    yes
O1 . Gd1 . O3 . 131.2(3)    yes
O2 . Gd1 . O3 . 67.1(3)    yes
O1 . Gd1 . O4 . 163.5(3)    yes
O2 . Gd1 . O4 . 127.9(3)    yes
O3 . Gd1 . O4 . 64.7(3)    yes
O1 . Gd1 . O5 . 92.7(4)    yes
O2 . Gd1 . O5 . 73.2(3)    yes
O3 . Gd1 . O5 . 85.0(3)    yes
O4 . Gd1 . O5 . 84.0(4)    yes
O1 . Gd1 . O6 . 78.5(3)    yes
O2 . Gd1 . O6 . 125.5(3)    yes
O3 . Gd1 . O6 . 142.2(3)    yes
O4 . Gd1 . O6 . 85.3(3)    yes
O5 . Gd1 . O6 . 68.7(3)    yes
O1 . Gd1 . O7 . 87.7(4)    yes
O2 . Gd1 . O7 . 141.7(3)    yes
O3 . Gd1 . O7 . 124.6(4)    yes
O4 . Gd1 . O7 . 84.1(4)    yes
O5 . Gd1 . O7 . 138.3(3)    yes
O1 . Gd1 . O8 . 80.3(3)    yes
O2 . Gd1 . O8 . 75.9(3)    yes
O3 . Gd1 . O8 . 77.2(3)    yes
O4 . Gd1 . O8 . 110.7(3)    yes
O5 . Gd1 . O8 . 148.5(3)    yes
O6 . Gd1 . O7 . 70.5(4)    yes
O6 . Gd1 . O8 . 137.7(3)    yes
O7 . Gd1 . O8 . 72.6(3)    yes
N1 . Ni1 . N9 . 90.9(4)    yes
N1 . Ni1 . N10 . 88.1(5)    yes
N9 . Ni1 . N10 . 98.6(5)    yes
N1 . Ni1 . O2 . 94.7(4)    yes
N9 . Ni1 . O2 . 91.7(4)    yes
N10 . Ni1 . O2 . 169.3(4)    yes
N1 . Ni1 . O3 . 90.1(4)    yes
N9 . Ni1 . O3 . 169.9(4)    yes
N10 . Ni1 . O3 . 91.5(4)    yes
O2 . Ni1 . O3 . 78.2(4)    yes
N1 . Ni1 . O9 . 178.8(4)    yes
N9 . Ni1 . O9 . 89.5(4)    yes
N10 . Ni1 . O9 . 90.7(4)    yes
O2 . Ni1 . O9 . 86.5(3)    yes
O3 . Ni1 . O9 . 89.7(3)    yes
W1 . C1 . N1 . 178.0(13)    yes
W1 . C2 . N2 . 175.8(15)    yes
W1 . C3 . N3 . 176.1(11)    yes
W1 . C4 . N4 . 174.8(13)    yes
W1 . C5 . N5 . 178.0(16)    yes
W1 . C6 . N6 . 178.5(13)    yes
W1 . C7 . N7 . 179.8(12)    yes
W1 . C8 . N8 . 175.5(12)    yes
O1 . C9 . H93 . 109.3    no
O1 . C9 . H92 . 110.3    no
H93 . C9 . H92 . 109.2    no
O1 . C9 . H91 . 109.0    no
H93 . C9 . H91 . 109.6    no
H92 . C9 . H91 . 109.5    no
C11 . C10 . C15 . 123.5(14)    yes
C11 . C10 . O1 . 124.6(13)    yes
C15 . C10 . O1 . 111.9(12)    yes
C10 . C11 . C12 . 118.9(15)    yes
C10 . C11 . H111 . 120.4    no
C12 . C11 . H111 . 120.7    no
C11 . C12 . C13 . 118.8(13)    yes
C11 . C12 . H121 . 120.5    no
C13 . C12 . H121 . 120.7    no
C12 . C13 . C14 . 123.0(14)    yes
C12 . C13 . H131 . 118.7    no
C14 . C13 . H131 . 118.3    no
C13 . C14 . C15 . 118.4(14)    yes
C13 . C14 . C16 . 118.0(13)    yes
C15 . C14 . C16 . 123.7(13)    yes
C14 . C15 . C10 . 117.3(12)    yes
C14 . C15 . O2 . 123.1(12)    yes
C10 . C15 . O2 . 119.5(12)    yes
C14 . C16 . N9 . 128.7(13)    yes
C14 . C16 . H161 . 115.9    no
N9 . C16 . H161 . 115.4    no
C18 . C17 . N9 . 111.2(12)    yes
C18 . C17 . H171 . 110.0    no
N9 . C17 . H171 . 109.0    no
C18 . C17 . H172 . 108.0    no
N9 . C17 . H172 . 109.1    no
H171 . C17 . H172 . 109.5    no
C17 . C18 . C19 . 115.4(15)    yes
C17 . C18 . H181 . 107.6    no
C19 . C18 . H181 . 108.0    no
C17 . C18 . H182 . 108.1    no
C19 . C18 . H182 . 108.0    no
H181 . C18 . H182 . 109.6    no
C18 . C19 . N10 . 114.4(13)    yes
C18 . C19 . H191 . 109.1    no
N10 . C19 . H191 . 108.0    no
C18 . C19 . H192 . 107.3    no
N10 . C19 . H192 . 108.4    no
H191 . C19 . H192 . 109.6    no
C21 . C20 . N10 . 127.0(12)    yes
C21 . C20 . H201 . 116.5    no
N10 . C20 . H201 . 116.5    no
C20 . C21 . C22 . 123.8(12)    yes
C20 . C21 . C23 . 116.7(12)    yes
C22 . C21 . C23 . 119.5(13)    yes
C21 . C22 . C26 . 117.6(11)    yes
C21 . C22 . O3 . 125.1(11)    yes
C26 . C22 . O3 . 117.4(11)    yes
C21 . C23 . C24 . 122.0(14)    yes
C21 . C23 . H231 . 119.0    no
C24 . C23 . H231 . 118.9    no
C23 . C24 . C25 . 120.2(14)    yes
C23 . C24 . H241 . 120.0    no
C25 . C24 . H241 . 119.8    no
C24 . C25 . C26 . 118.7(14)    yes
C24 . C25 . H251 . 120.9    no
C26 . C25 . H251 . 120.4    no
C22 . C26 . C25 . 122.0(13)    yes
C22 . C26 . O4 . 111.5(11)    yes
C25 . C26 . O4 . 126.6(12)    yes
O4 . C27 . H273 . 108.7    no
O4 . C27 . H272 . 109.7    no
H273 . C27 . H272 . 109.8    no
O4 . C27 . H271 . 108.9    no
H273 . C27 . H271 . 109.8    no
H272 . C27 . H271 . 109.9    no
Ni1 . N1 . C1 . 160.7(11)    yes
C17 . N9 . C16 . 119.7(12)    yes
C17 . N9 . Ni1 . 116.1(10)    yes
C16 . N9 . Ni1 . 124.2(9)    yes
C19 . N10 . C20 . 113.6(12)    yes
C19 . N10 . Ni1 . 122.3(10)    yes
C20 . N10 . Ni1 . 123.4(9)    yes
C9 . O1 . C10 . 115.6(11)    yes
C9 . O1 . Gd1 . 122.8(9)    yes
C10 . O1 . Gd1 . 119.2(8)    yes
C15 . O2 . Gd1 . 123.5(8)    yes
C15 . O2 . Ni1 . 126.6(8)    yes
Gd1 . O2 . Ni1 . 107.8(4)    yes
C22 . O3 . Ni1 . 121.5(8)    yes
C22 . O3 . Gd1 . 124.9(7)    yes
Ni1 . O3 . Gd1 . 106.9(4)    yes
C27 . O4 . C26 . 113.3(11)    yes
C27 . O4 . Gd1 . 125.8(8)    yes
C26 . O4 . Gd1 . 120.7(7)    yes
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C9 . H91 . N5 2_575 172.0 0.959 2.525 3.48(2)    yes
C12 . H121 . O8 1_455 147.0 0.929 2.552 3.37(2)    yes



 
data_shelx
 
_audit_creation_method            SHELXL-2014
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C27 H32 Dy N10 Ni O10 W' 
_chemical_formula_weight          1061.68

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Dy'  'Dy'  -0.1892   4.4098
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni'  'Ni'   0.3393   1.1124
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    8.9520(2)
_cell_length_b                    13.9264(3)
_cell_length_c                    27.3934(6)
_cell_angle_alpha                 90
_cell_angle_beta                  93.261(2)
_cell_angle_gamma                 90
_cell_volume                      3409.58(13)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     102111 
_cell_measurement_theta_min       2.09 
_cell_measurement_theta_max       33.82 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             green 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     2.068          
_exptl_crystal_F_000              2048
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.5 
_exptl_crystal_size_mid           0.35 
_exptl_crystal_size_min           0.25 
_exptl_absorpt_coefficient_mu     6.150
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.1232 
_exptl_absorpt_correction_T_max   0.2800 
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                       
_diffrn_measurement_device_type   'STOE-IPDS II' 
_diffrn_measurement_method        'omega scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             46283
_diffrn_reflns_av_unetI/netI      0.0455
_diffrn_reflns_av_R_equivalents   0.0949
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -36
_diffrn_reflns_limit_l_max        36
_diffrn_reflns_theta_min          2.087
_diffrn_reflns_theta_max          27.998
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.997
_diffrn_measured_fraction_theta_full  0.997
_diffrn_reflns_Laue_measured_fraction_max    0.997
_diffrn_reflns_Laue_measured_fraction_full   0.997
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.997
_reflns_number_total              8196
_reflns_number_gt                 7597
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'X-Area'
_computing_cell_refinement        'X-Area'
_computing_data_reduction         'X-Area'
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0464P)²+9.7041P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00071(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          8196
_refine_ls_number_parameters      476
_refine_ls_number_restraints      6
_refine_ls_R_factor_all           0.0454
_refine_ls_R_factor_gt            0.0413
_refine_ls_wR_factor_ref          0.1065
_refine_ls_wR_factor_gt           0.1033
_refine_ls_goodness_of_fit_ref    1.191
_refine_ls_restrained_S_all       1.190
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.6538(9) 0.3359(8) 0.0233(3) 0.062(3) Uani 1 1 d . . . . .
H1A H 0.6048 0.2892 0.0022 0.093 Uiso 1 1 calc R U . . .
H1B H 0.6694 0.3938 0.0053 0.093 Uiso 1 1 calc R U . . .
H1C H 0.7485 0.3111 0.0358 0.093 Uiso 1 1 calc R U . . .
C2 C 0.6200(6) 0.4239(4) 0.0974(2) 0.0282(11) Uani 1 1 d . . . . .
C3 C 0.7424(7) 0.4795(6) 0.0907(3) 0.0405(15) Uani 1 1 d . . . . .
H3 H 0.7929 0.4753 0.0621 0.049 Uiso 1 1 calc R U . . .
C4 C 0.7902(7) 0.5429(6) 0.1278(3) 0.0469(17) Uani 1 1 d . . . . .
H4 H 0.8735 0.5815 0.1239 0.056 Uiso 1 1 calc R U . . .
C5 C 0.7147(7) 0.5486(6) 0.1699(3) 0.0447(16) Uani 1 1 d . . . . .
H5 H 0.7477 0.5912 0.1943 0.054 Uiso 1 1 calc R U . . .
C6 C 0.5883(6) 0.4912(4) 0.1768(2) 0.0299(11) Uani 1 1 d . . . . .
C7 C 0.5388(5) 0.4269(4) 0.13983(19) 0.0229(10) Uani 1 1 d . . . . .
C8 C 0.5168(7) 0.5042(5) 0.2224(2) 0.0326(12) Uani 1 1 d . . . . .
H8 H 0.5695 0.5403 0.2462 0.039 Uiso 1 1 calc R U . . .
C9 C 0.3399(10) 0.5058(7) 0.2812(3) 0.054(2) Uani 1 1 d . . . . .
H9A H 0.4186 0.4929 0.3061 0.065 Uiso 1 1 calc R U . . .
H9B H 0.3266 0.5748 0.2795 0.065 Uiso 1 1 calc R U . . .
C10 C 0.2009(10) 0.4628(7) 0.2967(3) 0.058(2) Uani 1 1 d . . . . .
H10A H 0.1804 0.4886 0.3285 0.069 Uiso 1 1 calc R U . . .
H10B H 0.2163 0.3942 0.3005 0.069 Uiso 1 1 calc R U . . .
C11 C 0.0609(9) 0.4791(6) 0.2615(3) 0.0500(18) Uani 1 1 d . . . . .
H11A H -0.0289 0.4689 0.2790 0.060 Uiso 1 1 calc R U . . .
H11B H 0.0600 0.5448 0.2498 0.060 Uiso 1 1 calc R U . . .
C12 C -0.0589(6) 0.3652(5) 0.2092(2) 0.0336(13) Uani 1 1 d . . . . .
H12 H -0.1393 0.3765 0.2285 0.040 Uiso 1 1 calc R U . . .
C13 C -0.0823(6) 0.2957(5) 0.1705(2) 0.0312(12) Uani 1 1 d . . . . .
C14 C -0.2218(6) 0.2474(5) 0.1680(2) 0.0382(15) Uani 1 1 d . . . . .
H14 H -0.2922 0.2625 0.1905 0.046 Uiso 1 1 calc R U . . .
C15 C -0.2546(7) 0.1796(6) 0.1335(3) 0.0444(17) Uani 1 1 d . . . . .
H15 H -0.3471 0.1490 0.1328 0.053 Uiso 1 1 calc R U . . .
C16 C -0.1521(7) 0.1551(6) 0.0992(2) 0.0402(15) Uani 1 1 d . . . . .
H16 H -0.1746 0.1081 0.0758 0.048 Uiso 1 1 calc R U . . .
C17 C -0.0158(6) 0.2024(5) 0.1009(2) 0.0286(11) Uani 1 1 d . . . . .
C18 C 0.0201(6) 0.2728(4) 0.1359(2) 0.0276(11) Uani 1 1 d . . . . .
C19 C 0.0829(9) 0.0967(6) 0.0412(3) 0.0519(19) Uani 1 1 d . . . . .
H19A H 0.1653 0.0913 0.0204 0.078 Uiso 1 1 calc R U . . .
H19B H 0.0836 0.0430 0.0632 0.078 Uiso 1 1 calc R U . . .
H19C H -0.0093 0.0973 0.0215 0.078 Uiso 1 1 calc R U . . .
C20 C 0.2051(6) 0.6085(4) 0.13878(19) 0.0250(10) Uani 1 1 d . . . . .
C21 C 0.0793(6) 0.6760(4) 0.0621(2) 0.0279(11) Uani 1 1 d . . . . .
C22 C 0.0302(6) 0.7391(4) 0.1776(2) 0.0242(10) Uani 1 1 d . . . . .
C23 C -0.0171(6) 0.8369(5) 0.0992(2) 0.0319(12) Uani 1 1 d . . . . .
C24 C 0.2349(7) 0.9024(4) 0.1474(2) 0.0318(12) Uani 1 1 d . . . . .
C25 C 0.2337(7) 0.8427(5) 0.0568(2) 0.0325(12) Uani 1 1 d . . . . .
C26 C 0.4054(7) 0.7227(6) 0.0965(2) 0.0372(14) Uani 1 1 d . . . . .
C27 C 0.3344(6) 0.7500(4) 0.1866(2) 0.0270(11) Uani 1 1 d . . . . .
Dy1 Dy 0.32822(2) 0.27465(2) 0.07991(2) 0.02110(8) Uani 1 1 d . . . . .
N1 N 0.3906(6) 0.4722(4) 0.23366(17) 0.0303(10) Uani 1 1 d . . . . .
N2 N 0.0614(5) 0.4133(4) 0.21987(18) 0.0290(10) Uani 1 1 d . . . . .
N3 N 0.2139(5) 0.5295(4) 0.14796(18) 0.0293(10) Uani 1 1 d . . . . .
N4 N 0.0188(6) 0.6328(5) 0.0314(2) 0.0401(13) Uani 1 1 d . . . . .
N5 N -0.0524(6) 0.7291(4) 0.2069(2) 0.0371(12) Uani 1 1 d . . . . .
N6 N -0.1228(7) 0.8776(6) 0.0870(2) 0.0523(16) Uani 1 1 d . . . . .
N7 N 0.2654(8) 0.9782(5) 0.1583(3) 0.0533(16) Uani 1 1 d . . . . .
N8 N 0.2637(9) 0.8871(5) 0.0235(2) 0.0543(17) Uani 1 1 d . . . . .
N9 N 0.5215(7) 0.7106(7) 0.0826(3) 0.065(2) Uani 1 1 d . . . . .
N10 N 0.4191(7) 0.7470(5) 0.2195(2) 0.0448(14) Uani 1 1 d . . . . .
Ni1 Ni 0.25235(7) 0.39921(5) 0.18568(2) 0.02113(14) Uani 1 1 d . . . . .
O1 O 0.5617(4) 0.3564(4) 0.06351(15) 0.0337(9) Uani 1 1 d . . . . .
O2 O 0.4228(4) 0.3681(3) 0.14234(13) 0.0239(7) Uani 1 1 d . . . . .
O3 O 0.1527(4) 0.3160(3) 0.13338(13) 0.0233(7) Uani 1 1 d . . . . .
O4 O 0.0968(4) 0.1847(3) 0.06888(15) 0.0319(9) Uani 1 1 d . . . . .
O5 O 0.2101(6) 0.4202(4) 0.04860(19) 0.0460(12) Uani 1 1 d D . . . .
O6 O 0.2891(5) 0.2705(4) -0.00800(15) 0.0378(10) Uani 1 1 d . . . . .
O7 O 0.4541(7) 0.1377(4) 0.04849(19) 0.0512(13) Uani 1 1 d D . . . .
O8 O 0.3666(5) 0.1637(3) 0.14437(16) 0.0308(8) Uani 1 1 d D . . . .
O9 O 0.2997(4) 0.2633(3) 0.22766(14) 0.0271(8) Uani 1 1 d . . . . .
O10 O 0.5848(9) 0.9615(7) 0.0703(7) 0.185(8) Uani 1 1 d . . . . .
W1 W 0.18758(2) 0.75945(2) 0.12094(2) 0.01832(8) Uani 1 1 d . . . . .
H7W H 0.357(8) 0.197(5) 0.1689(17) 0.04(2) Uiso 1 1 d D . . . .
H8W H 0.336(8) 0.109(2) 0.149(3) 0.04(2) Uiso 1 1 d D . . . .
H1W H 0.159(7) 0.434(6) 0.0239(16) 0.04(2) Uiso 1 1 d D . . . .
H6W H 0.489(10) 0.086(3) 0.058(3) 0.06(3) Uiso 1 1 d D . . . .
H2W H 0.201(12) 0.444(8) 0.0757(18) 0.09(4) Uiso 1 1 d D . . . .
H5W H 0.451(9) 0.123(6) 0.0195(8) 0.05(2) Uiso 1 1 d D . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.440(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.362(8) . ?
C2 O1 1.400(7) . ?
C2 C7 1.407(7) . ?
C3 C4 1.394(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.408(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.404(8) . ?
C6 C8 1.445(9) . ?
C7 O2 1.328(6) . ?
C8 N1 1.269(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.466(11) . ?
C9 N1 1.478(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.554(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.462(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N2 1.288(8) . ?
C12 C13 1.441(10) . ?
C12 H12 0.9300 . ?
C13 C18 1.392(8) . ?
C13 C14 1.417(8) . ?
C14 C15 1.357(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.392(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.386(7) . ?
C16 H16 0.9300 . ?
C17 O4 1.396(7) . ?
C17 C18 1.396(8) . ?
C18 O3 1.336(6) . ?
C19 O4 1.443(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N3 1.130(8) . ?
C20 W1 2.162(6) . ?
C21 N4 1.146(8) . ?
C21 W1 2.170(6) . ?
C22 N5 1.131(8) . ?
C22 W1 2.172(5) . ?
C23 N6 1.136(8) . ?
C23 W1 2.180(5) . ?
C24 N7 1.127(9) . ?
C24 W1 2.152(6) . ?
C25 N8 1.147(9) . ?
C25 W1 2.163(6) . ?
C26 N9 1.139(9) . ?
C26 W1 2.159(6) . ?
C27 N10 1.145(8) . ?
C27 W1 2.170(5) . ?
Dy1 O2 2.274(4) . ?
Dy1 O3 2.282(4) . ?
Dy1 O8 2.357(4) . ?
Dy1 O7 2.400(5) . ?
Dy1 O6 2.414(4) . ?
Dy1 O5 2.420(5) . ?
Dy1 O4 2.425(4) . ?
Dy1 O1 2.444(4) . ?
Dy1 Ni1 3.4768(7) . ?
N1 Ni1 2.027(5) . ?
N2 Ni1 2.005(5) . ?
N3 Ni1 2.106(5) . ?
Ni1 O3 2.011(4) . ?
Ni1 O2 2.033(4) . ?
Ni1 O9 2.242(4) . ?
O5 H1W 0.820(5) . ?
O5 H2W 0.820(5) . ?
O7 H6W 0.820(5) . ?
O7 H5W 0.820(5) . ?
O8 H7W 0.821(5) . ?
O8 H8W 0.820(5) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O1 124.4(5) . . ?
C3 C2 C7 123.4(6) . . ?
O1 C2 C7 112.2(5) . . ?
C2 C3 C4 118.6(6) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 120.3(6) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.2(6) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 119.1(6) . . ?
C7 C6 C8 124.5(5) . . ?
C5 C6 C8 116.4(5) . . ?
O2 C7 C6 124.8(5) . . ?
O2 C7 C2 117.8(5) . . ?
C6 C7 C2 117.4(5) . . ?
N1 C8 C6 127.6(5) . . ?
N1 C8 H8 116.2 . . ?
C6 C8 H8 116.2 . . ?
C10 C9 N1 115.7(6) . . ?
C10 C9 H9A 108.3 . . ?
N1 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
N1 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 115.4(7) . . ?
C9 C10 H10A 108.4 . . ?
C11 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
C11 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
N2 C11 C10 110.7(6) . . ?
N2 C11 H11A 109.5 . . ?
C10 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
N2 C12 C13 126.9(5) . . ?
N2 C12 H12 116.5 . . ?
C13 C12 H12 116.5 . . ?
C18 C13 C14 118.1(6) . . ?
C18 C13 C12 125.5(5) . . ?
C14 C13 C12 116.4(6) . . ?
C15 C14 C13 121.3(6) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 121.0(6) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C17 C16 C15 118.3(6) . . ?
C17 C16 H16 120.8 . . ?
C15 C16 H16 120.8 . . ?
C16 C17 O4 124.2(6) . . ?
C16 C17 C18 121.6(6) . . ?
O4 C17 C18 114.2(5) . . ?
O3 C18 C13 123.6(5) . . ?
O3 C18 C17 116.8(5) . . ?
C13 C18 C17 119.6(5) . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 W1 179.7(6) . . ?
N4 C21 W1 178.4(5) . . ?
N5 C22 W1 179.5(6) . . ?
N6 C23 W1 178.7(6) . . ?
N7 C24 W1 175.1(6) . . ?
N8 C25 W1 177.3(6) . . ?
N9 C26 W1 174.7(8) . . ?
N10 C27 W1 175.6(6) . . ?
O2 Dy1 O3 67.25(13) . . ?
O2 Dy1 O8 77.26(15) . . ?
O3 Dy1 O8 76.17(15) . . ?
O2 Dy1 O7 124.22(17) . . ?
O3 Dy1 O7 141.74(18) . . ?
O8 Dy1 O7 72.32(17) . . ?
O2 Dy1 O6 142.23(16) . . ?
O3 Dy1 O6 125.46(14) . . ?
O8 Dy1 O6 137.59(16) . . ?
O7 Dy1 O6 70.59(18) . . ?
O2 Dy1 O5 85.64(16) . . ?
O3 Dy1 O5 73.33(17) . . ?
O8 Dy1 O5 148.93(17) . . ?
O7 Dy1 O5 137.99(18) . . ?
O6 Dy1 O5 68.33(17) . . ?
O2 Dy1 O4 131.94(13) . . ?
O3 Dy1 O4 66.17(14) . . ?
O8 Dy1 O4 80.89(15) . . ?
O7 Dy1 O4 87.69(19) . . ?
O6 Dy1 O4 77.82(15) . . ?
O5 Dy1 O4 92.03(18) . . ?
O2 Dy1 O1 65.54(13) . . ?
O3 Dy1 O1 128.87(14) . . ?
O8 Dy1 O1 110.71(15) . . ?
O7 Dy1 O1 83.2(2) . . ?
O6 Dy1 O1 84.53(15) . . ?
O5 Dy1 O1 84.59(18) . . ?
O4 Dy1 O1 162.01(14) . . ?
O2 Dy1 Ni1 33.87(9) . . ?
O3 Dy1 Ni1 33.38(9) . . ?
O8 Dy1 Ni1 74.32(11) . . ?
O7 Dy1 Ni1 144.43(13) . . ?
O6 Dy1 Ni1 144.98(12) . . ?
O5 Dy1 Ni1 77.02(13) . . ?
O4 Dy1 Ni1 98.96(10) . . ?
O1 Dy1 Ni1 97.49(10) . . ?
C8 N1 C9 115.2(5) . . ?
C8 N1 Ni1 122.5(4) . . ?
C9 N1 Ni1 121.5(4) . . ?
C12 N2 C11 117.6(5) . . ?
C12 N2 Ni1 124.5(4) . . ?
C11 N2 Ni1 117.8(4) . . ?
C20 N3 Ni1 162.7(5) . . ?
N2 Ni1 O3 91.93(18) . . ?
N2 Ni1 N1 98.8(2) . . ?
O3 Ni1 N1 168.70(18) . . ?
N2 Ni1 O2 169.11(18) . . ?
O3 Ni1 O2 77.20(14) . . ?
N1 Ni1 O2 91.99(17) . . ?
N2 Ni1 N3 91.4(2) . . ?
O3 Ni1 N3 95.35(18) . . ?
N1 Ni1 N3 87.9(2) . . ?
O2 Ni1 N3 90.25(18) . . ?
N2 Ni1 O9 89.10(18) . . ?
O3 Ni1 O9 86.69(15) . . ?
N1 Ni1 O9 90.02(18) . . ?
O2 Ni1 O9 89.62(15) . . ?
N3 Ni1 O9 177.87(18) . . ?
N2 Ni1 Dy1 130.56(15) . . ?
O3 Ni1 Dy1 38.63(10) . . ?
N1 Ni1 Dy1 130.51(14) . . ?
O2 Ni1 Dy1 38.57(10) . . ?
N3 Ni1 Dy1 93.16(14) . . ?
O9 Ni1 Dy1 88.06(10) . . ?
C2 O1 C1 115.5(5) . . ?
C2 O1 Dy1 118.8(3) . . ?
C1 O1 Dy1 125.5(4) . . ?
C7 O2 Ni1 120.9(3) . . ?
C7 O2 Dy1 125.0(3) . . ?
Ni1 O2 Dy1 107.55(15) . . ?
C18 O3 Ni1 125.6(3) . . ?
C18 O3 Dy1 124.5(4) . . ?
Ni1 O3 Dy1 107.98(15) . . ?
C17 O4 C19 115.9(5) . . ?
C17 O4 Dy1 118.2(3) . . ?
C19 O4 Dy1 123.5(4) . . ?
Dy1 O5 H1W 135(6) . . ?
Dy1 O5 H2W 95(8) . . ?
H1W O5 H2W 125(10) . . ?
Dy1 O7 H6W 140(7) . . ?
Dy1 O7 H5W 124(6) . . ?
H6W O7 H5W 95(8) . . ?
Dy1 O8 H7W 103(6) . . ?
Dy1 O8 H8W 134(5) . . ?
H7W O8 H8W 109(8) . . ?
C24 W1 C26 99.2(3) . . ?
C24 W1 C20 144.4(2) . . ?
C26 W1 C20 77.5(2) . . ?
C24 W1 C25 74.6(2) . . ?
C26 W1 C25 70.0(2) . . ?
C20 W1 C25 133.6(2) . . ?
C24 W1 C21 144.7(2) . . ?
C26 W1 C21 90.9(2) . . ?
C20 W1 C21 70.8(2) . . ?
C25 W1 C21 77.4(2) . . ?
C24 W1 C27 71.3(2) . . ?
C26 W1 C27 74.2(2) . . ?
C20 W1 C27 73.8(2) . . ?
C25 W1 C27 124.8(2) . . ?
C21 W1 C27 143.8(2) . . ?
C24 W1 C22 90.2(2) . . ?
C26 W1 C22 145.5(2) . . ?
C20 W1 C22 75.7(2) . . ?
C25 W1 C22 144.2(2) . . ?
C21 W1 C22 100.4(2) . . ?
C27 W1 C22 77.7(2) . . ?
C24 W1 C23 77.3(2) . . ?
C26 W1 C23 142.4(2) . . ?
C20 W1 C23 126.3(2) . . ?
C25 W1 C23 73.1(2) . . ?
C21 W1 C23 74.2(2) . . ?
C27 W1 C23 135.8(2) . . ?
C22 W1 C23 72.0(2) . . ?
 
_refine_diff_density_max    2.665
_refine_diff_density_min   -3.743
_refine_diff_density_rms    0.203

_shelxl_version_number 2014-3



 
data_shelx
 
_audit_creation_method            SHELXL-2014
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C27 H32 Lu N10 Ni O10 W' 
_chemical_formula_weight          1074.15

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Lu'  'Lu'  -0.4720   5.8584
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni'  'Ni'   0.3393   1.1124
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            19
_space_group_name_H-M_alt         'P 21 21 21'
_space_group_name_Hall            'P 2ac 2ab'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 
_cell_length_a                    8.9298(4)
_cell_length_b                    13.9422(7)
_cell_length_c                    30.8112(19)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      3836.0(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     26423 
_cell_measurement_theta_min       2.29 
_cell_measurement_theta_max       30.80 
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             green 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.860          
_exptl_crystal_F_000              2068
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.2 
_exptl_crystal_size_mid           0.08 
_exptl_crystal_size_min           0.04 
_exptl_absorpt_coefficient_mu     6.092
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4766
_exptl_absorpt_correction_T_max   0.6352
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                       
_diffrn_measurement_device_type   'STOE-IPDS II' 
_diffrn_measurement_method        'omega scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             19721
_diffrn_reflns_av_unetI/netI      0.0738
_diffrn_reflns_av_R_equivalents   0.0947
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -40
_diffrn_reflns_limit_l_max        40
_diffrn_reflns_theta_min          2.375
_diffrn_reflns_theta_max          27.995
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.914
_diffrn_measured_fraction_theta_full  0.886
_diffrn_reflns_Laue_measured_fraction_max    0.914
_diffrn_reflns_Laue_measured_fraction_full   0.886
_diffrn_reflns_point_group_measured_fraction_max   0.929
_diffrn_reflns_point_group_measured_fraction_full  0.906
_reflns_number_total              7808
_reflns_number_gt                 6462
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.818
_reflns_Friedel_fraction_max      0.949
_reflns_Friedel_fraction_full     0.931
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'X-Area'
_computing_cell_refinement        'X-Area'
_computing_data_reduction         'X-Area'
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1597P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0113(11)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.13(4)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          7808
_refine_ls_number_parameters      453
_refine_ls_number_restraints      14
_refine_ls_R_factor_all           0.0984
_refine_ls_R_factor_gt            0.0840
_refine_ls_wR_factor_ref          0.2316
_refine_ls_wR_factor_gt           0.2182
_refine_ls_goodness_of_fit_ref    1.055
_refine_ls_restrained_S_all       1.055
_refine_ls_shift/su_max           0.003
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.326(4) 0.049(3) 0.9538(9) 0.079(12) Uani 1 1 d . . . . .
H1A H 0.3780 -0.0005 0.9696 0.119 Uiso 1 1 calc R U . . .
H1B H 0.3126 0.1037 0.9721 0.119 Uiso 1 1 calc R U . . .
H1C H 0.2306 0.0253 0.9445 0.119 Uiso 1 1 calc R U . . .
C2 C 0.353(3) 0.1473(19) 0.8900(11) 0.052(7) Uani 1 1 d . . . . .
C3 C 0.218(3) 0.194(2) 0.8989(14) 0.063(9) Uani 1 1 d . . . . .
H3 H 0.1597 0.1815 0.9233 0.076 Uiso 1 1 calc R U . . .
C4 C 0.178(4) 0.266(3) 0.8655(15) 0.081(13) Uani 1 1 d . . . . .
H4 H 0.0881 0.2993 0.8690 0.098 Uiso 1 1 calc R U . . .
C5 C 0.259(4) 0.286(2) 0.8317(14) 0.068(10) Uani 1 1 d . . . . .
H5 H 0.2330 0.3371 0.8140 0.081 Uiso 1 1 calc R U . . .
C6 C 0.388(3) 0.230(3) 0.8212(10) 0.057(8) Uani 1 1 d . . . . .
C7 C 0.434(4) 0.156(2) 0.8528(9) 0.051(7) Uani 1 1 d . . . . .
C8 C 0.461(4) 0.256(3) 0.7823(13) 0.073(11) Uani 1 1 d . . . . .
H8 H 0.4137 0.3007 0.7647 0.088 Uiso 1 1 calc R U . . .
C9 C 0.625(5) 0.260(3) 0.7249(16) 0.079(13) Uani 1 1 d . . . . .
H9A H 0.6300 0.3292 0.7256 0.094 Uiso 1 1 calc R U . . .
H9B H 0.5469 0.2415 0.7046 0.094 Uiso 1 1 calc R U . . .
C10 C 0.779(4) 0.218(2) 0.7090(13) 0.065(9) Uani 1 1 d . . . . .
H10A H 0.7690 0.1495 0.7060 0.078 Uiso 1 1 calc R U . . .
H10B H 0.7994 0.2442 0.6804 0.078 Uiso 1 1 calc R U . . .
C11 C 0.909(4) 0.238(3) 0.7367(11) 0.065(9) Uani 1 1 d . . . . .
H11A H 0.9023 0.3032 0.7474 0.078 Uiso 1 1 calc R U . . .
H11B H 0.9993 0.2334 0.7192 0.078 Uiso 1 1 calc R U . . .
C12 C 1.040(3) 0.124(2) 0.7793(11) 0.053(6) Uani 1 1 d . . . . .
H12 H 1.1155 0.1349 0.7591 0.064 Uiso 1 1 calc R U . . .
C13 C 1.070(3) 0.056(2) 0.8124(9) 0.047(6) Uani 1 1 d . . . . .
C14 C 1.212(3) 0.008(2) 0.8124(9) 0.049(5) Uani 1 1 d . . . . .
H14 H 1.2826 0.0241 0.7916 0.058 Uiso 1 1 calc R U . . .
C15 C 1.246(3) -0.063(3) 0.8423(11) 0.058(7) Uani 1 1 d . . . . .
H15 H 1.3371 -0.0950 0.8402 0.070 Uiso 1 1 calc R U . . .
C16 C 1.145(3) -0.090(2) 0.8764(15) 0.070(10) Uani 1 1 d . . . . .
H16 H 1.1686 -0.1355 0.8972 0.084 Uiso 1 1 calc R U . . .
C17 C 1.004(4) -0.0393(19) 0.8759(9) 0.050(6) Uani 1 1 d . . . . .
C18 C 0.975(3) 0.0332(17) 0.8438(11) 0.049(7) Uani 1 1 d . . . . .
C19 C 0.930(4) -0.145(3) 0.9331(14) 0.071(10) Uani 1 1 d . . . . .
H19A H 0.8438 -0.1539 0.9513 0.106 Uiso 1 1 calc R U . . .
H19B H 0.9482 -0.2023 0.9167 0.106 Uiso 1 1 calc R U . . .
H19C H 1.0158 -0.1312 0.9509 0.106 Uiso 1 1 calc R U . . .
C20 C 0.776(3) 0.353(2) 0.8494(9) 0.045(6) Uani 1 1 d . . . . .
C21 C 0.961(4) 0.486(2) 0.8178(10) 0.058(7) Uani 1 1 d . . . . .
C22 C 0.897(4) 0.415(2) 0.9202(9) 0.051(6) Uani 1 1 d . . . . .
C23 C 1.009(4) 0.589(3) 0.8878(10) 0.058(7) Uani 1 1 d . . . . .
C24 C 0.759(6) 0.578(7) 0.9300(18) 0.15(3) Uani 1 1 d . . . . .
C25 C 0.773(4) 0.652(2) 0.8452(10) 0.054(7) Uani 1 1 d . . . . .
C26 C 0.574(5) 0.482(4) 0.895(2) 0.139(18) Uani 1 1 d D U . . .
C27 C 0.646(4) 0.514(2) 0.8154(10) 0.073(8) Uani 1 1 d D U . . .
Lu1 Lu 0.65955(11) 0.01658(8) 0.89751(3) 0.0413(3) Uani 1 1 d . . . . .
N1 N 0.587(3) 0.2226(18) 0.7693(7) 0.048(5) Uani 1 1 d . . . . .
N2 N 0.923(3) 0.1707(16) 0.7749(9) 0.052(6) Uani 1 1 d . . . . .
N3 N 0.762(2) 0.2855(18) 0.8401(7) 0.044(5) Uani 1 1 d . . . . .
N4 N 1.047(3) 0.480(2) 0.7901(9) 0.061(7) Uani 1 1 d . . . . .
N5 N 0.941(4) 0.371(2) 0.9481(10) 0.069(8) Uani 1 1 d . . . . .
N6 N 1.109(4) 0.620(3) 0.8990(18) 0.100(14) Uani 1 1 d . . . . .
N7 N 0.735(4) 0.6382(18) 0.9571(10) 0.071(9) Uani 1 1 d . . . . .
N8 N 0.766(9) 0.734(3) 0.8379(14) 0.15(3) Uani 1 1 d . . . . .
N9 N 0.475(4) 0.445(3) 0.910(2) 0.129(17) Uani 1 1 d D U . . .
N10 N 0.566(4) 0.515(3) 0.7875(10) 0.077(8) Uani 1 1 d D U . . .
Ni1 Ni 0.7306(4) 0.1523(2) 0.80734(11) 0.0399(7) Uani 1 1 d . . . . .
O1 O 0.413(2) 0.0757(17) 0.9165(7) 0.055(5) Uani 1 1 d . . . . .
O2 O 0.561(2) 0.1086(15) 0.8469(5) 0.046(4) Uani 1 1 d . . . . .
O3 O 0.836(2) 0.0724(11) 0.8526(5) 0.039(3) Uani 1 1 d . . . . .
O4 O 0.903(2) -0.0625(18) 0.9025(8) 0.063(6) Uani 1 1 d . . . . .
O5 O 0.722(3) 0.1665(15) 0.9251(7) 0.067(7) Uani 1 1 d . . . . .
O6 O 0.687(3) 0.000(2) 0.9745(7) 0.077(7) Uani 1 1 d . . . . .
O7 O 0.552(3) -0.1217(17) 0.9188(8) 0.066(6) Uani 1 1 d . . . . .
O8 O 0.637(3) -0.0815(15) 0.8380(7) 0.053(5) Uani 1 1 d . . . . .
O9 O 0.696(2) 0.0138(14) 0.7666(5) 0.047(4) Uani 1 1 d . . . . .
O10 O 0.789(5) 0.123(3) 1.0303(11) 0.103(11) Uani 1 1 d . . . . .
W1 W 0.80111(10) 0.50880(7) 0.86987(3) 0.0418(3) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 O1 1.44(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C7 1.36(4) . ?
C2 C3 1.40(3) . ?
C2 O1 1.40(4) . ?
C3 C4 1.48(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.30(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.43(4) . ?
C5 H5 0.9300 . ?
C6 C8 1.41(5) . ?
C6 C7 1.48(4) . ?
C7 O2 1.33(3) . ?
C8 N1 1.28(5) . ?
C8 H8 0.9300 . ?
C9 N1 1.50(4) . ?
C9 C10 1.57(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.47(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.51(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N2 1.23(4) . ?
C12 C13 1.42(5) . ?
C12 H12 0.9300 . ?
C13 C18 1.32(4) . ?
C13 C14 1.44(3) . ?
C14 C15 1.39(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.43(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.44(3) . ?
C16 H16 0.9300 . ?
C17 O4 1.26(4) . ?
C17 C18 1.44(4) . ?
C18 O3 1.38(3) . ?
C19 O4 1.51(4) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N3 0.99(3) . ?
C20 W1 2.28(3) . ?
C21 N4 1.16(4) . ?
C21 W1 2.17(3) . ?
C22 N5 1.13(4) . ?
C22 W1 2.20(3) . ?
C23 N6 1.06(5) . ?
C23 W1 2.23(3) . ?
C24 N7 1.21(8) . ?
C24 W1 2.12(7) . ?
C25 N8 1.17(5) . ?
C25 W1 2.15(3) . ?
C26 N9 1.122(7) . ?
C26 W1 2.21(3) . ?
C27 N10 1.122(7) . ?
C27 W1 2.17(2) . ?
Lu1 O2 2.201(18) . ?
Lu1 O3 2.236(16) . ?
Lu1 O7 2.25(2) . ?
Lu1 O8 2.30(2) . ?
Lu1 O5 2.32(2) . ?
Lu1 O6 2.397(19) . ?
Lu1 O1 2.42(2) . ?
Lu1 O4 2.44(2) . ?
Lu1 Ni1 3.421(3) . ?
N1 Ni1 2.00(2) . ?
N2 Ni1 2.01(2) . ?
N3 Ni1 2.13(3) . ?
Ni1 O3 2.019(17) . ?
Ni1 O2 2.03(2) . ?
Ni1 O9 2.32(2) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C2 C3 126(3) . . ?
C7 C2 O1 110(2) . . ?
C3 C2 O1 124(3) . . ?
C2 C3 C4 113(3) . . ?
C2 C3 H3 123.5 . . ?
C4 C3 H3 123.5 . . ?
C5 C4 C3 124(3) . . ?
C5 C4 H4 117.9 . . ?
C3 C4 H4 117.9 . . ?
C4 C5 C6 121(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C8 C6 C5 115(3) . . ?
C8 C6 C7 128(3) . . ?
C5 C6 C7 117(3) . . ?
O2 C7 C2 122(3) . . ?
O2 C7 C6 120(3) . . ?
C2 C7 C6 118(2) . . ?
N1 C8 C6 125(3) . . ?
N1 C8 H8 117.3 . . ?
C6 C8 H8 117.3 . . ?
N1 C9 C10 111(3) . . ?
N1 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C9 116(3) . . ?
C11 C10 H10A 108.2 . . ?
C9 C10 H10A 108.2 . . ?
C11 C10 H10B 108.2 . . ?
C9 C10 H10B 108.2 . . ?
H10A C10 H10B 107.3 . . ?
C10 C11 N2 114(3) . . ?
C10 C11 H11A 108.8 . . ?
N2 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
N2 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
N2 C12 C13 126(3) . . ?
N2 C12 H12 117.0 . . ?
C13 C12 H12 117.0 . . ?
C18 C13 C12 125(3) . . ?
C18 C13 C14 117(3) . . ?
C12 C13 C14 119(3) . . ?
C15 C14 C13 122(3) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C14 C15 C16 122(3) . . ?
C14 C15 H15 118.9 . . ?
C16 C15 H15 118.9 . . ?
C15 C16 C17 115(3) . . ?
C15 C16 H16 122.6 . . ?
C17 C16 H16 122.6 . . ?
O4 C17 C18 120(2) . . ?
O4 C17 C16 120(3) . . ?
C18 C17 C16 120(3) . . ?
C13 C18 O3 128(3) . . ?
C13 C18 C17 124(3) . . ?
O3 C18 C17 108(2) . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C20 W1 178(3) . . ?
N4 C21 W1 176(3) . . ?
N5 C22 W1 175(3) . . ?
N6 C23 W1 173(4) . . ?
N7 C24 W1 163(6) . . ?
N8 C25 W1 170(3) . . ?
N9 C26 W1 161(5) . . ?
N10 C27 W1 179(3) . . ?
O2 Lu1 O3 68.9(7) . . ?
O2 Lu1 O7 122.4(9) . . ?
O3 Lu1 O7 141.2(8) . . ?
O2 Lu1 O8 75.4(7) . . ?
O3 Lu1 O8 77.0(7) . . ?
O7 Lu1 O8 71.7(8) . . ?
O2 Lu1 O5 80.2(8) . . ?
O3 Lu1 O5 75.2(8) . . ?
O7 Lu1 O5 140.0(8) . . ?
O8 Lu1 O5 148.1(7) . . ?
O2 Lu1 O6 143.0(8) . . ?
O3 Lu1 O6 124.9(8) . . ?
O7 Lu1 O6 70.9(9) . . ?
O8 Lu1 O6 137.9(9) . . ?
O5 Lu1 O6 72.5(9) . . ?
O2 Lu1 O1 67.1(7) . . ?
O3 Lu1 O1 132.1(7) . . ?
O7 Lu1 O1 80.4(9) . . ?
O8 Lu1 O1 108.5(8) . . ?
O5 Lu1 O1 79.7(9) . . ?
O6 Lu1 O1 83.6(8) . . ?
O2 Lu1 O4 131.5(8) . . ?
O3 Lu1 O4 64.5(8) . . ?
O7 Lu1 O4 88.6(10) . . ?
O8 Lu1 O4 81.9(9) . . ?
O5 Lu1 O4 99.8(10) . . ?
O6 Lu1 O4 78.6(9) . . ?
O1 Lu1 O4 161.3(8) . . ?
O2 Lu1 Ni1 34.5(5) . . ?
O3 Lu1 Ni1 34.4(5) . . ?
O7 Lu1 Ni1 142.1(6) . . ?
O8 Lu1 Ni1 72.4(5) . . ?
O5 Lu1 Ni1 75.8(5) . . ?
O6 Lu1 Ni1 146.9(7) . . ?
O1 Lu1 Ni1 100.1(5) . . ?
O4 Lu1 Ni1 97.8(6) . . ?
C8 N1 C9 111(3) . . ?
C8 N1 Ni1 124(2) . . ?
C9 N1 Ni1 124(2) . . ?
C12 N2 C11 119(3) . . ?
C12 N2 Ni1 127(2) . . ?
C11 N2 Ni1 113.3(19) . . ?
C20 N3 Ni1 169(2) . . ?
N1 Ni1 N2 101.4(11) . . ?
N1 Ni1 O3 167.7(9) . . ?
N2 Ni1 O3 90.9(9) . . ?
N1 Ni1 O2 91.2(9) . . ?
N2 Ni1 O2 166.8(9) . . ?
O3 Ni1 O2 76.5(7) . . ?
N1 Ni1 N3 86.3(10) . . ?
N2 Ni1 N3 90.7(9) . . ?
O3 Ni1 N3 95.3(8) . . ?
O2 Ni1 N3 94.2(8) . . ?
N1 Ni1 O9 90.3(9) . . ?
N2 Ni1 O9 87.1(8) . . ?
O3 Ni1 O9 88.6(7) . . ?
O2 Ni1 O9 88.7(7) . . ?
N3 Ni1 O9 175.6(7) . . ?
N1 Ni1 Lu1 129.0(8) . . ?
N2 Ni1 Lu1 129.4(8) . . ?
O3 Ni1 Lu1 38.7(5) . . ?
O2 Ni1 Lu1 37.8(5) . . ?
N3 Ni1 Lu1 97.0(6) . . ?
O9 Ni1 Lu1 87.4(4) . . ?
C2 O1 C1 116(3) . . ?
C2 O1 Lu1 117.1(16) . . ?
C1 O1 Lu1 127(2) . . ?
C7 O2 Ni1 124.7(18) . . ?
C7 O2 Lu1 122.2(16) . . ?
Ni1 O2 Lu1 107.7(8) . . ?
C18 O3 Ni1 120.0(16) . . ?
C18 O3 Lu1 128.1(14) . . ?
Ni1 O3 Lu1 106.9(8) . . ?
C17 O4 C19 119(2) . . ?
C17 O4 Lu1 118.7(17) . . ?
C19 O4 Lu1 122(2) . . ?
C24 W1 C25 82(2) . . ?
C24 W1 C21 146.0(19) . . ?
C25 W1 C21 87.2(13) . . ?
C24 W1 C27 123(2) . . ?
C25 W1 C27 67.9(11) . . ?
C21 W1 C27 81.4(14) . . ?
C24 W1 C22 74(2) . . ?
C25 W1 C22 147.5(11) . . ?
C21 W1 C22 100.3(11) . . ?
C27 W1 C22 144.2(10) . . ?
C24 W1 C26 67(3) . . ?
C25 W1 C26 99.9(18) . . ?
C21 W1 C26 147(2) . . ?
C27 W1 C26 72(2) . . ?
C22 W1 C26 90.6(19) . . ?
C24 W1 C23 72.8(18) . . ?
C25 W1 C23 73.7(14) . . ?
C21 W1 C23 73.2(12) . . ?
C27 W1 C23 134.6(12) . . ?
C22 W1 C23 78.3(12) . . ?
C26 W1 C23 139(2) . . ?
C24 W1 C20 131(2) . . ?
C25 W1 C20 141.1(10) . . ?
C21 W1 C20 73.8(12) . . ?
C27 W1 C20 75.8(11) . . ?
C22 W1 C20 70.6(10) . . ?
C26 W1 C20 81.3(19) . . ?
C23 W1 C20 129.0(12) . . ?
 
_refine_diff_density_max    3.956
_refine_diff_density_min   -1.685
_refine_diff_density_rms    0.324

_shelxl_version_number 2014-3



