# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Mn2
_database_code_depnum_ccdc_archive 'CCDC 1883422'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H9 Mn2 N5 O48 P2 W12'
_chemical_formula_weight         3873.57

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_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, -z'
'-x, y, -z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'

_cell_length_a                   19.1135(2)
_cell_length_b                   28.3342(3)
_cell_length_c                   25.0357(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13558.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    10009
_cell_measurement_theta_min      1.521
_cell_measurement_theta_max      29.502

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_F_000             6916
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    10.395
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10077
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.521
_diffrn_reflns_theta_max         29.502
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.533
_diffrn_reflns_point_group_measured_fraction_full 0.539
_reflns_number_total             10077
_reflns_number_gt                8619
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.000
_reflns_Friedel_fraction_full    0.000

_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       'Rigaku CrystalClear'
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.0844P)²+56.8792P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.08(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10077
_refine_ls_number_parameters     397
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1299
_refine_ls_wR_factor_gt          0.1248
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.002
_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
P1 P 0.60165(10) 0.64259(7) 0.74906(12) 0.0228(4) Uani 1 1 d . . . . .
W1 W 0.40207(3) 0.64006(2) 0.60885(2) 0.03129(13) Uani 1 1 d . . . . .
W2 W 0.75383(3) 0.67243(3) 0.81527(2) 0.03619(16) Uani 1 1 d . . . . .
W3 W 0.75239(3) 0.67203(3) 0.68274(2) 0.03894(17) Uani 1 1 d . . . . .
W4 W 0.59476(3) 0.63968(3) 0.60758(2) 0.03213(14) Uani 1 1 d . . . . .
W5 W 0.40134(3) 0.74520(2) 0.67597(2) 0.02828(13) Uani 1 1 d . . . . .
W6 W 0.59835(3) 0.74488(2) 0.67327(2) 0.02922(13) Uani 1 1 d . . . . .
Mn1 Mn 0.49946(14) 0.56818(5) 0.68914(5) 0.0314(3) Uani 1 1 d . . . . .
O1 O 0.4226(5) 0.5819(4) 0.6340(3) 0.034(2) Uani 1 1 d . . . . .
O2 O 0.5777(5) 0.5830(4) 0.6336(4) 0.041(3) Uani 1 1 d . . . . .
O3 O 0.5736(3) 0.5927(2) 0.7485(4) 0.0285(12) Uani 1 1 d . . . . .
O4 O 0.3766(5) 0.6314(5) 0.5432(4) 0.045(3) Uani 1 1 d . . . . .
O5 O 0.8207(6) 0.6851(6) 0.8574(4) 0.064(4) Uani 1 1 d . . . . .
O6 O 0.8205(4) 0.6882(4) 0.6401(4) 0.040(3) Uani 1 1 d . . . . .
O7 O 0.6165(5) 0.6278(5) 0.5431(4) 0.051(3) Uani 1 1 d . . . . .
O8 O 0.4967(5) 0.6553(3) 0.5994(2) 0.0363(15) Uani 1 1 d . . . . .
O9 O 0.3052(5) 0.6389(4) 0.6403(3) 0.034(2) Uani 1 1 d . . . . .
O10 O 0.7988(3) 0.6874(3) 0.7480(5) 0.0422(17) Uani 1 1 d . . . . .
O11 O 0.6914(5) 0.6424(5) 0.6357(4) 0.042(3) Uani 1 1 d . . . . .
O12 O 0.6830(3) 0.6431(2) 0.7493(4) 0.0314(13) Uani 1 1 d . . . . .
O13 O 0.4221(4) 0.6672(4) 0.7006(3) 0.029(2) Uani 1 1 d . . . . .
O14 O 0.5766(4) 0.6683(3) 0.6969(3) 0.0219(16) Uani 1 1 d . . . . .
O15 O 0.3947(5) 0.7107(4) 0.6126(3) 0.040(3) Uani 1 1 d . . . . .
O16 O 0.2996(4) 0.7238(4) 0.6867(3) 0.035(2) Uani 1 1 d . . . . .
O17 O 0.6993(4) 0.7262(4) 0.6819(4) 0.035(2) Uani 1 1 d . . . . .
O18 O 0.6059(5) 0.7099(3) 0.6108(3) 0.0296(19) Uani 1 1 d . . . . .
O19 O 0.5006(5) 0.7489(2) 0.6724(2) 0.0310(13) Uani 1 1 d . . . . .
O20 O 0.4017(3) 0.7539(2) 0.7502(3) 0.0294(13) Uani 1 1 d . . . . .
O21 O 0.3805(5) 0.8016(4) 0.6528(4) 0.039(2) Uani 1 1 d . . . . .
O22 O 0.6154(5) 0.7996(5) 0.6529(4) 0.051(3) Uani 1 1 d . . . . .
N201 N 0.7984(6) 0.6040(5) 0.7020(4) 0.035(3) Uiso 1 1 d . . . . .
O201 O 0.7970(6) 0.6059(5) 0.7947(5) 0.050(3) Uiso 1 1 d . . . . .
C201 C 0.8119(7) 0.5854(4) 0.7481(10) 0.053(3) Uiso 1 1 d . . . . .
C202 C 0.8487(10) 0.5401(5) 0.7433(10) 0.080(5) Uiso 1 1 d . . . . .
H20A H 0.8577 0.5276 0.7782 0.121 Uiso 1 1 calc R U . . .
H20B H 0.8203 0.5183 0.7235 0.121 Uiso 1 1 calc R U . . .
H20C H 0.8923 0.5448 0.7249 0.121 Uiso 1 1 calc R U . . .
C101 C 0.5000 0.4763(5) 0.7500 0.062(4) Uiso 1 2 d DS . P . .
C102 C 0.5000 0.4216(5) 0.7500 0.138(13) Uiso 1 2 d DS . P . .
H10A H 0.5046 0.4103 0.7140 0.208 Uiso 0.5 1 calc R U P . .
H10B H 0.5385 0.4103 0.7710 0.208 Uiso 0.5 1 calc R U P . .
H10C H 0.4569 0.4103 0.7649 0.208 Uiso 0.5 1 calc R U P . .
O101 O 0.5057(7) 0.4962(3) 0.7053(3) 0.052(2) Uiso 1 1 d . . . . .
N1 N 0.7813(9) 0.7081(6) 0.4898(7) 0.073(3) Uiso 1 1 d . U . . .
C111 C 0.8549(11) 0.7276(7) 0.4785(8) 0.074(4) Uiso 1 1 d . U . . .
C112 C 0.9026(12) 0.7290(9) 0.5292(10) 0.090(5) Uiso 1 1 d . U . . .
C113 C 0.9769(14) 0.7465(9) 0.5125(11) 0.106(6) Uiso 1 1 d . U . . .
C114 C 1.0119(19) 0.7161(11) 0.4777(13) 0.145(10) Uiso 1 1 d . U . . .
C121 C 0.7755(12) 0.6640(8) 0.5178(9) 0.083(5) Uiso 1 1 d . U . . .
C122 C 0.8065(16) 0.6238(8) 0.4892(12) 0.122(7) Uiso 1 1 d D U . . .
C123 C 0.790(2) 0.5730(8) 0.5083(16) 0.147(8) Uiso 1 1 d D U . . .
C124 C 0.821(3) 0.5543(16) 0.547(2) 0.203(14) Uiso 1 1 d . U . . .
C131 C 0.7472(10) 0.7438(7) 0.5262(8) 0.071(4) Uiso 1 1 d . U . . .
C132 C 0.7358(13) 0.7864(8) 0.5055(12) 0.099(6) Uiso 1 1 d D U . . .
C133 C 0.7199(16) 0.8213(7) 0.5496(12) 0.118(7) Uiso 1 1 d D U . . .
C134 C 0.701(2) 0.8710(7) 0.5280(14) 0.180(13) Uiso 1 1 d D U . . .
C141 C 0.7465(10) 0.7140(8) 0.4363(9) 0.082(5) Uiso 1 1 d . U . . .
C142 C 0.6706(14) 0.6977(9) 0.4387(11) 0.109(6) Uiso 1 1 d D U . . .
C143 C 0.6325(18) 0.7070(8) 0.3816(14) 0.143(8) Uiso 1 1 d D U . . .
C144 C 0.609(2) 0.7592(9) 0.3814(17) 0.237(16) Uiso 1 1 d D U . . .
N2 N 0.5000 0.9044(5) 0.7500 0.060(3) Uiso 1 2 d S U P . .
C211 C 0.5623(8) 0.8725(5) 0.7544(8) 0.062(3) Uiso 1 1 d . U . . .
C212 C 0.6362(10) 0.9002(7) 0.7369(8) 0.079(4) Uiso 1 1 d . U . . .
C213 C 0.6990(11) 0.8707(7) 0.7410(10) 0.084(5) Uiso 1 1 d . U . . .
C214 C 0.7611(13) 0.8934(9) 0.7321(11) 0.102(7) Uiso 1 1 d . U . . .
C221 C 0.4923(14) 0.9358(6) 0.7059(8) 0.083(4) Uiso 1 1 d . U . . .
C222 C 0.4949(18) 0.9105(8) 0.6500(10) 0.109(5) Uiso 1 1 d . U . . .
C223 C 0.516(2) 0.9495(11) 0.6091(14) 0.149(8) Uiso 1 1 d . U . . .
C224 C 0.491(3) 0.9343(14) 0.557(2) 0.211(14) Uiso 1 1 d . U . . .


_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
P1 O13 1.511(8) 3_656 ?
P1 O3 1.511(6) . ?
P1 O12 1.555(6) . ?
P1 O14 1.569(8) . ?
W1 O4 1.731(8) . ?
W1 O1 1.807(11) . ?
W1 O8 1.874(10) . ?
W1 O15 2.008(13) . ?
W1 O9 2.012(10) . ?
W1 O13 2.452(8) . ?
W2 O5 1.695(11) . ?
W2 O16 1.780(12) 3_656 ?
W2 O9 1.848(10) 3_656 ?
W2 O10 1.936(11) . ?
W2 O201 2.120(13) . ?
W2 O12 2.292(9) . ?
W3 O6 1.745(8) . ?
W3 O17 1.841(11) . ?
W3 O11 1.858(10) . ?
W3 O10 1.910(11) . ?
W3 N201 2.173(13) . ?
W3 O12 2.281(9) . ?
W4 O7 1.701(10) . ?
W4 O2 1.763(12) . ?
W4 O8 1.936(10) . ?
W4 O11 1.978(9) . ?
W4 O18 2.004(9) . ?
W4 O14 2.404(7) . ?
W5 O21 1.746(10) . ?
W5 O15 1.869(10) . ?
W5 O20 1.875(8) . ?
W5 O19 1.902(10) . ?
W5 O16 2.054(10) . ?
W5 O13 2.328(11) . ?
W6 O22 1.665(14) . ?
W6 O18 1.857(9) . ?
W6 O19 1.873(10) . ?
W6 O20 1.932(8) 3_656 ?
W6 O17 2.012(8) . ?
W6 O14 2.289(9) . ?
Mn1 O1 2.054(9) . ?
Mn1 O2 2.085(10) . ?
Mn1 O101 2.083(8) . ?
Mn1 O3 2.169(8) . ?
Mn1 O3 2.207(9) 3_656 ?
Mn1 Mn1 3.047(3) 3_656 ?
O3 Mn1 2.207(9) 3_656 ?
O9 W2 1.848(10) 3_656 ?
O13 P1 1.511(8) 3_656 ?
O16 W2 1.780(12) 3_656 ?
O20 W6 1.932(8) 3_656 ?
N201 C201 1.30(2) . ?
O201 C201 1.34(2) . ?
C201 C202 1.467(19) . ?
C202 H20A 0.9600 . ?
C202 H20B 0.9600 . ?
C202 H20C 0.9600 . ?
C101 O101 1.258(11) 3_656 ?
C101 O101 1.258(11) . ?
C101 C102 1.5500(10) . ?
C102 H10A 0.9600 . ?
C102 H10B 0.9600 . ?
C102 H10C 0.9600 . ?
N1 C121 1.44(3) . ?
N1 C131 1.51(3) . ?
N1 C141 1.51(3) . ?
N1 C111 1.54(2) . ?
C111 C112 1.56(3) . ?
C112 C113 1.56(3) . ?
C113 C114 1.40(4) . ?
C121 C122 1.47(3) . ?
C122 C123 1.5501(10) . ?
C123 C124 1.25(5) . ?
C131 C132 1.33(3) . ?
C132 C133 1.51(3) . ?
C133 C134 1.5500(10) . ?
C141 C142 1.52(3) . ?
C142 C143 1.63(4) . ?
C143 C144 1.5501(10) . ?
N2 C221 1.42(2) . ?
N2 C221 1.42(2) 3_656 ?
N2 C211 1.499(17) 3_656 ?
N2 C211 1.499(17) . ?
C211 C212 1.68(2) . ?
C212 C213 1.47(3) . ?
C213 C214 1.37(3) . ?
C221 C222 1.57(3) . ?
C222 C223 1.56(4) . ?
C223 C224 1.45(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
O13 P1 O3 109.4(6) 3_656 . ?
O13 P1 O12 107.1(5) 3_656 . ?
O3 P1 O12 111.3(3) . . ?
O13 P1 O14 112.8(3) 3_656 . ?
O3 P1 O14 108.6(5) . . ?
O12 P1 O14 107.6(5) . . ?
O4 W1 O1 105.2(5) . . ?
O4 W1 O8 100.6(4) . . ?
O1 W1 O8 92.5(4) . . ?
O4 W1 O15 99.5(5) . . ?
O1 W1 O15 155.2(4) . . ?
O8 W1 O15 81.1(4) . . ?
O4 W1 O9 96.3(4) . . ?
O1 W1 O9 92.8(4) . . ?
O8 W1 O9 160.2(3) . . ?
O15 W1 O9 86.2(4) . . ?
O4 W1 O13 167.8(5) . . ?
O1 W1 O13 85.8(4) . . ?
O8 W1 O13 84.0(3) . . ?
O15 W1 O13 69.8(3) . . ?
O9 W1 O13 77.4(3) . . ?
O5 W2 O16 106.0(6) . 3_656 ?
O5 W2 O9 101.2(5) . 3_656 ?
O16 W2 O9 95.0(4) 3_656 3_656 ?
O5 W2 O10 99.2(4) . . ?
O16 W2 O10 93.0(4) 3_656 . ?
O9 W2 O10 155.0(4) 3_656 . ?
O5 W2 O201 92.6(6) . . ?
O16 W2 O201 160.7(4) 3_656 . ?
O9 W2 O201 85.8(5) 3_656 . ?
O10 W2 O201 79.1(4) . . ?
O5 W2 O12 166.1(5) . . ?
O16 W2 O12 86.4(3) 3_656 . ?
O9 W2 O12 83.5(4) 3_656 . ?
O10 W2 O12 73.4(3) . . ?
O201 W2 O12 74.6(3) . . ?
O6 W3 O17 100.7(5) . . ?
O6 W3 O11 101.4(5) . . ?
O17 W3 O11 91.4(5) . . ?
O6 W3 O10 96.8(4) . . ?
O17 W3 O10 94.4(4) . . ?
O11 W3 O10 159.6(4) . . ?
O6 W3 N201 93.8(5) . . ?
O17 W3 N201 164.9(4) . . ?
O11 W3 N201 89.7(5) . . ?
O10 W3 N201 79.8(4) . . ?
O6 W3 O12 167.1(4) . . ?
O17 W3 O12 89.2(3) . . ?
O11 W3 O12 86.4(4) . . ?
O10 W3 O12 74.1(3) . . ?
N201 W3 O12 75.8(3) . . ?
O7 W4 O2 102.5(6) . . ?
O7 W4 O8 100.5(4) . . ?
O2 W4 O8 93.9(4) . . ?
O7 W4 O11 96.7(4) . . ?
O2 W4 O11 94.4(5) . . ?
O8 W4 O11 158.8(4) . . ?
O7 W4 O18 102.0(5) . . ?
O2 W4 O18 155.5(4) . . ?
O8 W4 O18 83.1(3) . . ?
O11 W4 O18 81.2(5) . . ?
O7 W4 O14 170.1(5) . . ?
O2 W4 O14 86.4(4) . . ?
O8 W4 O14 83.2(3) . . ?
O11 W4 O14 77.9(3) . . ?
O18 W4 O14 69.1(3) . . ?
O21 W5 O15 100.4(5) . . ?
O21 W5 O20 102.1(4) . . ?
O15 W5 O20 155.6(4) . . ?
O21 W5 O19 99.3(4) . . ?
O15 W5 O19 93.3(4) . . ?
O20 W5 O19 92.0(3) . . ?
O21 W5 O16 95.6(4) . . ?
O15 W5 O16 83.8(4) . . ?
O20 W5 O16 85.0(3) . . ?
O19 W5 O16 165.1(4) . . ?
O21 W5 O13 174.6(4) . . ?
O15 W5 O13 74.9(4) . . ?
O20 W5 O13 82.0(3) . . ?
O19 W5 O13 84.0(3) . . ?
O16 W5 O13 81.2(4) . . ?
O22 W6 O18 102.9(5) . . ?
O22 W6 O19 97.7(4) . . ?
O18 W6 O19 95.8(3) . . ?
O22 W6 O20 100.4(4) . 3_656 ?
O18 W6 O20 154.9(3) . 3_656 ?
O19 W6 O20 90.1(3) . 3_656 ?
O22 W6 O17 95.2(5) . . ?
O18 W6 O17 82.9(4) . . ?
O19 W6 O17 167.0(4) . . ?
O20 W6 O17 85.9(3) 3_656 . ?
O22 W6 O14 177.0(4) . . ?
O18 W6 O14 74.1(3) . . ?
O19 W6 O14 83.1(3) . . ?
O20 W6 O14 82.4(3) 3_656 . ?
O17 W6 O14 84.1(4) . . ?
O1 Mn1 O2 91.5(3) . . ?
O1 Mn1 O101 110.9(5) . . ?
O2 Mn1 O101 106.6(5) . . ?
O1 Mn1 O3 150.2(3) . . ?
O2 Mn1 O3 85.6(4) . . ?
O101 Mn1 O3 98.2(4) . . ?
O1 Mn1 O3 87.9(3) . 3_656 ?
O2 Mn1 O3 149.6(3) . 3_656 ?
O101 Mn1 O3 102.0(4) . 3_656 ?
O3 Mn1 O3 80.1(2) . 3_656 ?
O1 Mn1 Mn1 132.6(3) . 3_656 ?
O2 Mn1 Mn1 131.5(3) . 3_656 ?
O101 Mn1 Mn1 78.8(2) . 3_656 ?
O3 Mn1 Mn1 46.4(3) . 3_656 ?
O3 Mn1 Mn1 45.4(2) 3_656 3_656 ?
W1 O1 Mn1 124.2(5) . . ?
W4 O2 Mn1 124.2(5) . . ?
P1 O3 Mn1 122.5(5) . . ?
P1 O3 Mn1 120.9(5) . 3_656 ?
Mn1 O3 Mn1 88.3(2) . 3_656 ?
W1 O8 W4 150.2(4) . . ?
W2 O9 W1 142.0(6) 3_656 . ?
W3 O10 W2 119.2(3) . . ?
W3 O11 W4 146.0(7) . . ?
P1 O12 W3 125.7(5) . . ?
P1 O12 W2 126.6(6) . . ?
W3 O12 W2 93.0(2) . . ?
P1 O13 W5 127.5(5) 3_656 . ?
P1 O13 W1 126.1(6) 3_656 . ?
W5 O13 W1 91.3(3) . . ?
P1 O14 W6 126.9(5) . . ?
P1 O14 W4 125.0(5) . . ?
W6 O14 W4 93.0(3) . . ?
W5 O15 W1 123.8(5) . . ?
W2 O16 W5 141.4(6) 3_656 . ?
W3 O17 W6 138.5(6) . . ?
W6 O18 W4 123.7(4) . . ?
W6 O19 W5 172.5(4) . . ?
W5 O20 W6 164.9(4) . 3_656 ?
C201 N201 W3 129.8(10) . . ?
C201 O201 W2 133.1(11) . . ?
N201 C201 O201 123.9(10) . . ?
N201 C201 C202 112(2) . . ?
O201 C201 C202 124(2) . . ?
C201 C202 H20A 109.5 . . ?
C201 C202 H20B 109.5 . . ?
H20A C202 H20B 109.5 . . ?
C201 C202 H20C 109.5 . . ?
H20A C202 H20C 109.5 . . ?
H20B C202 H20C 109.5 . . ?
O101 C101 O101 126.7(15) 3_656 . ?
O101 C101 C102 116.6(7) 3_656 . ?
O101 C101 C102 116.6(7) . . ?
C101 C102 H10A 109.5 . . ?
C101 C102 H10B 109.5 . . ?
H10A C102 H10B 109.5 . . ?
C101 C102 H10C 109.5 . . ?
H10A C102 H10C 109.5 . . ?
H10B C102 H10C 109.5 . . ?
C101 O101 Mn1 127.3(8) . . ?
C121 N1 C131 104.7(16) . . ?
C121 N1 C141 119.8(17) . . ?
C131 N1 C141 105.8(15) . . ?
C121 N1 C111 118.3(17) . . ?
C131 N1 C111 105.4(15) . . ?
C141 N1 C111 101.6(15) . . ?
N1 C111 C112 113.1(16) . . ?
C113 C112 C111 108.7(19) . . ?
C114 C113 C112 114(2) . . ?
N1 C121 C122 113.9(19) . . ?
C121 C122 C123 119(2) . . ?
C124 C123 C122 122(4) . . ?
C132 C131 N1 116(2) . . ?
C131 C132 C133 110(2) . . ?
C132 C133 C134 112.6(19) . . ?
C142 C141 N1 110.6(19) . . ?
C141 C142 C143 110(2) . . ?
C144 C143 C142 106.7(19) . . ?
C221 N2 C221 102.8(19) . 3_656 ?
C221 N2 C211 103.8(12) . 3_656 ?
C221 N2 C211 121.1(12) 3_656 3_656 ?
C221 N2 C211 121.1(12) . . ?
C221 N2 C211 103.8(12) 3_656 . ?
C211 N2 C211 105.7(14) 3_656 . ?
N2 C211 C212 111.5(12) . . ?
C213 C212 C211 113.8(16) . . ?
C214 C213 C212 115.4(19) . . ?
N2 C221 C222 113.7(16) . . ?
C221 C222 C223 106(2) . . ?
C224 C223 C222 107(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 W1 O1 Mn1 146.5(5) . . . . ?
O8 W1 O1 Mn1 44.8(5) . . . . ?
O15 W1 O1 Mn1 -29.3(13) . . . . ?
O9 W1 O1 Mn1 -116.2(5) . . . . ?
O13 W1 O1 Mn1 -39.0(5) . . . . ?
O7 W4 O2 Mn1 -143.3(6) . . . . ?
O8 W4 O2 Mn1 -41.7(6) . . . . ?
O11 W4 O2 Mn1 118.8(6) . . . . ?
O18 W4 O2 Mn1 40.3(13) . . . . ?
O14 W4 O2 Mn1 41.2(6) . . . . ?
O13 P1 O3 Mn1 115.7(6) 3_656 . . . ?
O12 P1 O3 Mn1 -126.2(5) . . . . ?
O14 P1 O3 Mn1 -7.9(6) . . . . ?
O13 P1 O3 Mn1 5.9(6) 3_656 . . 3_656 ?
O12 P1 O3 Mn1 124.0(5) . . . 3_656 ?
O14 P1 O3 Mn1 -117.7(5) . . . 3_656 ?
O4 W1 O8 W4 -111.6(9) . . . . ?
O1 W1 O8 W4 -5.7(8) . . . . ?
O15 W1 O8 W4 150.3(8) . . . . ?
O9 W1 O8 W4 99.7(14) . . . . ?
O13 W1 O8 W4 79.8(8) . . . . ?
O6 W3 O11 W4 -126.4(12) . . . . ?
O17 W3 O11 W4 -25.2(12) . . . . ?
O10 W3 O11 W4 81(2) . . . . ?
N201 W3 O11 W4 139.8(12) . . . . ?
O12 W3 O11 W4 64.0(12) . . . . ?
O13 P1 O12 W3 -125.1(6) 3_656 . . . ?
O3 P1 O12 W3 115.3(6) . . . . ?
O14 P1 O12 W3 -3.6(7) . . . . ?
O13 P1 O12 W2 2.8(7) 3_656 . . . ?
O3 P1 O12 W2 -116.8(6) . . . . ?
O14 P1 O12 W2 124.3(5) . . . . ?
O13 P1 O14 W6 57.1(5) 3_656 . . . ?
O3 P1 O14 W6 178.6(4) . . . . ?
O12 P1 O14 W6 -60.8(6) . . . . ?
O13 P1 O14 W4 -175.6(6) 3_656 . . . ?
O3 P1 O14 W4 -54.2(6) . . . . ?
O12 P1 O14 W4 66.5(6) . . . . ?
O21 W5 O15 W1 -173.3(6) . . . . ?
O20 W5 O15 W1 -15.6(13) . . . . ?
O19 W5 O15 W1 86.6(6) . . . . ?
O16 W5 O15 W1 -78.8(6) . . . . ?
O13 W5 O15 W1 3.8(5) . . . . ?
O6 W3 O17 W6 132.7(8) . . . . ?
O11 W3 O17 W6 30.8(8) . . . . ?
O10 W3 O17 W6 -129.5(8) . . . . ?
N201 W3 O17 W6 -63(2) . . . . ?
O12 W3 O17 W6 -55.5(8) . . . . ?
O22 W6 O18 W4 177.7(6) . . . . ?
O19 W6 O18 W4 -82.9(5) . . . . ?
O20 W6 O18 W4 19.8(11) 3_656 . . . ?
O17 W6 O18 W4 84.0(6) . . . . ?
O14 W6 O18 W4 -1.8(5) . . . . ?
O21 W5 O20 W6 165.5(13) . . . 3_656 ?
O15 W5 O20 W6 7.9(18) . . . 3_656 ?
O19 W5 O20 W6 -94.6(13) . . . 3_656 ?
O16 W5 O20 W6 70.8(13) . . . 3_656 ?
O13 W5 O20 W6 -11.0(13) . . . 3_656 ?
W3 N201 C201 O201 1.9(18) . . . . ?
W3 N201 C201 C202 -175.2(11) . . . . ?
W2 O201 C201 N201 -3(2) . . . . ?
W2 O201 C201 C202 173.6(12) . . . . ?
O101 C101 O101 Mn1 -5.5(7) 3_656 . . . ?
C102 C101 O101 Mn1 174.5(7) . . . . ?
C121 N1 C111 C112 -50(2) . . . . ?
C131 N1 C111 C112 66(2) . . . . ?
C141 N1 C111 C112 176.2(18) . . . . ?
N1 C111 C112 C113 176.7(17) . . . . ?
C111 C112 C113 C114 -64(3) . . . . ?
C131 N1 C121 C122 -180(2) . . . . ?
C141 N1 C121 C122 62(3) . . . . ?
C111 N1 C121 C122 -63(3) . . . . ?
N1 C121 C122 C123 -167(3) . . . . ?
C121 C122 C123 C124 -81(5) . . . . ?
C121 N1 C131 C132 -170(2) . . . . ?
C141 N1 C131 C132 -42(3) . . . . ?
C111 N1 C131 C132 65(2) . . . . ?
N1 C131 C132 C133 -165.0(19) . . . . ?
C131 C132 C133 C134 -176(3) . . . . ?
C121 N1 C141 C142 49(3) . . . . ?
C131 N1 C141 C142 -69(2) . . . . ?
C111 N1 C141 C142 -178.4(17) . . . . ?
N1 C141 C142 C143 176.9(17) . . . . ?
C141 C142 C143 C144 -83(3) . . . . ?
C221 N2 C211 C212 41(2) . . . . ?
C221 N2 C211 C212 -73.0(17) 3_656 . . . ?
C211 N2 C211 C212 158.7(18) 3_656 . . . ?
N2 C211 C212 C213 179.3(16) . . . . ?
C211 C212 C213 C214 -174(2) . . . . ?
C221 N2 C221 C222 171(3) 3_656 . . . ?
C211 N2 C221 C222 -63(2) 3_656 . . . ?
C211 N2 C221 C222 56(3) . . . . ?
N2 C221 C222 C223 -158(2) . . . . ?
C221 C222 C223 C224 -156(3) . . . . ?

_refine_diff_density_max         1.675
_refine_diff_density_min         -2.124
_refine_diff_density_rms         0.389

_shelxl_version_number           2014/6





loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.101 -0.002 -0.002 5472 4213 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Cu2
_database_code_depnum_ccdc_archive 'CCDC 1883425'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H9 Cu2 N5 O48 P2 W12'
_chemical_formula_weight         3890.88

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_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, -z'
'-x, y, -z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'

_cell_length_a                   19.0981(2)
_cell_length_b                   28.4851(3)
_cell_length_c                   24.8371(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13511.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9885
_cell_measurement_theta_min      1.284
_cell_measurement_theta_max      29.421

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale plue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_F_000             6912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    10.559
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9948
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.284
_diffrn_reflns_theta_max         29.421
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.531
_diffrn_reflns_point_group_measured_fraction_full 0.539
_reflns_number_total             9948
_reflns_number_gt                8520
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.000
_reflns_Friedel_fraction_full    0.000

_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       'Rigaku CrystalClear'
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1138P)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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.066(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9948
_refine_ls_number_parameters     402
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1574
_refine_ls_wR_factor_gt          0.1536
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.143
_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
P1 P 0.39923(10) 0.64251(7) 0.25095(11) 0.0292(4) Uani 1 1 d . . . . .
W1 W 0.59638(3) 0.63829(2) 0.39071(2) 0.04095(14) Uani 1 1 d . . . . .
W2 W 0.24701(2) 0.66997(3) 0.18446(2) 0.04601(17) Uani 1 1 d . . . . .
W3 W 0.24829(2) 0.67065(3) 0.31776(2) 0.04666(17) Uani 1 1 d . . . . .
W4 W 0.40615(3) 0.63886(2) 0.39211(2) 0.04149(15) Uani 1 1 d . . . . .
W5 W 0.59903(3) 0.74319(2) 0.32481(2) 0.03680(13) Uani 1 1 d . . . . .
W6 W 0.40214(3) 0.74368(2) 0.32702(2) 0.03771(13) Uani 1 1 d . . . . .
Cu1 Cu 0.49997(10) 0.57603(4) 0.30821(5) 0.0403(2) Uani 1 1 d . . . . .
O1 O 0.5732(4) 0.5825(3) 0.3616(3) 0.045(2) Uani 1 1 d . . . . .
O2 O 0.4310(5) 0.5853(4) 0.3632(3) 0.051(2) Uani 1 1 d . . . . .
O3 O 0.5702(3) 0.5928(2) 0.2498(4) 0.0396(12) Uani 1 1 d . . . . .
O4 O 0.6221(5) 0.6238(4) 0.4553(3) 0.060(3) Uani 1 1 d . . . . .
O5 O 0.1774(4) 0.6858(4) 0.1393(4) 0.052(2) Uani 1 1 d . . . . .
O6 O 0.1829(5) 0.6813(6) 0.3602(4) 0.088(5) Uani 1 1 d . . . . .
O7 O 0.3831(4) 0.6298(5) 0.4584(3) 0.063(3) Uani 1 1 d . . . . .
O8 O 0.5012(4) 0.6548(3) 0.4028(2) 0.0446(15) Uani 1 1 d . . . . .
O9 O 0.6953(4) 0.6366(5) 0.3588(3) 0.057(3) Uani 1 1 d . . . . .
O10 O 0.2020(3) 0.6857(3) 0.2518(4) 0.0497(18) Uani 1 1 d . . . . .
O11 O 0.3100(4) 0.6396(3) 0.3655(3) 0.0391(19) Uani 1 1 d . . . . .
O12 O 0.3181(3) 0.6423(2) 0.2515(3) 0.0386(13) Uani 1 1 d . . . . .
O13 O 0.5769(3) 0.6649(3) 0.3004(3) 0.0348(18) Uani 1 1 d . . . . .
O14 O 0.4239(4) 0.6696(3) 0.3026(3) 0.0266(14) Uani 1 1 d . . . . .
O15 O 0.6059(4) 0.7084(4) 0.3882(3) 0.047(2) Uani 1 1 d . . . . .
O16 O 0.7015(5) 0.7220(4) 0.3150(3) 0.054(3) Uani 1 1 d . . . . .
O17 O 0.3025(3) 0.7231(4) 0.3173(3) 0.045(2) Uani 1 1 d . . . . .
O18 O 0.3955(4) 0.7080(4) 0.3899(3) 0.047(2) Uani 1 1 d . . . . .
O19 O 0.5008(4) 0.7479(2) 0.3290(2) 0.0365(13) Uani 1 1 d . . . . .
O20 O 0.4030(3) 0.7534(2) 0.2489(3) 0.0426(16) Uani 1 1 d . . . . .
O21 O 0.6209(4) 0.7983(4) 0.3487(4) 0.055(3) Uani 1 1 d . . . . .
O22 O 0.3828(5) 0.7981(4) 0.3486(4) 0.061(3) Uani 1 1 d . . . . .
O101 O 0.4940(7) 0.5032(3) 0.2945(4) 0.071(2) Uani 1 1 d . U . . .
C101 C 0.5000 0.4841(6) 0.2500 0.074(3) Uiso 1 2 d DS U P . .
C102 C 0.5000 0.4328(7) 0.2500 0.123(7) Uiso 1 2 d DS U P . .
H10A H 0.5049 0.4216 0.2138 0.184 Uiso 0.5 1 calc R U P . .
H10B H 0.5384 0.4216 0.2714 0.184 Uiso 0.5 1 calc R U P . .
H10C H 0.4567 0.4216 0.2649 0.184 Uiso 0.5 1 calc R U P . .
O201 O 0.2035(5) 0.6034(4) 0.2079(4) 0.053(2) Uiso 1 1 d . . . . .
N201 N 0.2035(6) 0.6034(4) 0.3024(4) 0.049(3) Uiso 1 1 d . . . . .
N1 N 0.2182(10) 0.7141(8) 0.5074(9) 0.109(3) Uiso 1 1 d . U . . .
C111 C 0.2300(12) 0.6618(7) 0.4805(9) 0.106(4) Uiso 1 1 d D U . . .
C112 C 0.1986(11) 0.6236(6) 0.5179(9) 0.117(4) Uiso 1 1 d D U . . .
C113 C 0.2044(12) 0.5752(8) 0.4822(10) 0.121(5) Uiso 1 1 d D U . . .
C114 C 0.2505(13) 0.5411(7) 0.5155(12) 0.151(8) Uiso 1 1 d D U . . .
C121 C 0.1425(11) 0.7257(8) 0.5216(9) 0.101(4) Uiso 1 1 d . U . . .
C122 C 0.0983(11) 0.7284(9) 0.4672(9) 0.102(4) Uiso 1 1 d . U . . .
C123 C 0.0167(11) 0.7431(8) 0.4904(10) 0.110(5) Uiso 1 1 d . U . . .
C124 C -0.0125(13) 0.7106(9) 0.5228(10) 0.122(6) Uiso 1 1 d . U . . .
C131 C 0.2574(12) 0.7286(10) 0.5598(12) 0.119(4) Uiso 1 1 d . U . . .
C132 C 0.3370(15) 0.7075(10) 0.5583(8) 0.129(5) Uiso 1 1 d D U . . .
C133 C 0.3706(12) 0.7098(8) 0.6155(9) 0.126(5) Uiso 1 1 d D U . . .
C134 C 0.3351(13) 0.6739(8) 0.6536(8) 0.127(7) Uiso 1 1 d D U . . .
C141 C 0.2528(14) 0.7480(6) 0.4738(11) 0.113(4) Uiso 1 1 d D U . . .
C142 C 0.2544(12) 0.7955(6) 0.4927(10) 0.133(5) Uiso 1 1 d D U . . .
C143 C 0.2817(16) 0.8337(6) 0.4535(8) 0.156(6) Uiso 1 1 d D U . . .
C144 C 0.2870(18) 0.8819(6) 0.4821(12) 0.182(9) Uiso 1 1 d D U . . .
N2 N 0.5000 0.9019(8) 0.2500 0.095(4) Uiso 1 2 d S U P . .
C201 C 0.1903(9) 0.5825(5) 0.2503(10) 0.076(3) Uiso 1 1 d . U . . .
C202 C 0.1504(10) 0.5408(5) 0.2611(7) 0.082(4) Uiso 1 1 d . U . . .
H20A H 0.1509 0.5345 0.2991 0.123 Uiso 1 1 calc R U . . .
H20B H 0.1029 0.5454 0.2494 0.123 Uiso 1 1 calc R U . . .
H20C H 0.1705 0.5148 0.2421 0.123 Uiso 1 1 calc R U . . .
C211 C 0.4389(10) 0.8718(7) 0.2446(9) 0.095(3) Uiso 1 1 d . U . . .
C212 C 0.3654(8) 0.8980(7) 0.2635(9) 0.099(4) Uiso 1 1 d D U . . .
C213 C 0.2990(9) 0.8710(7) 0.2376(9) 0.103(4) Uiso 1 1 d D U . . .
C214 C 0.2320(7) 0.8947(8) 0.2601(12) 0.143(7) Uiso 1 1 d D U . . .
C221 C 0.5077(14) 0.9343(7) 0.2929(6) 0.113(4) Uiso 1 1 d D U . . .
C222 C 0.5118(13) 0.9137(6) 0.3505(6) 0.128(5) Uiso 1 1 d D U . . .
C223 C 0.5154(11) 0.9528(6) 0.3938(8) 0.143(6) Uiso 1 1 d D U . . .
C224 C 0.4616(13) 0.9431(11) 0.4392(8) 0.169(8) Uiso 1 1 d D U . . .


_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
P1 O13 1.497(7) 3_655 ?
P1 O3 1.532(7) 3_655 ?
P1 O12 1.549(6) . ?
P1 O14 1.570(7) . ?
W1 O4 1.727(8) . ?
W1 O1 1.802(11) . ?
W1 O8 1.901(8) . ?
W1 O15 2.005(11) . ?
W1 O9 2.049(9) . ?
W1 O13 2.397(7) . ?
W2 O16 1.779(12) 3_655 ?
W2 O5 1.796(9) . ?
W2 O9 1.809(9) 3_655 ?
W2 O10 1.932(10) . ?
W2 O201 2.150(11) . ?
W2 O12 2.290(8) . ?
W3 O6 1.662(9) . ?
W3 O17 1.818(9) . ?
W3 O11 1.892(8) . ?
W3 O10 1.911(10) . ?
W3 N201 2.131(13) . ?
W3 O12 2.267(7) . ?
W4 O7 1.724(8) . ?
W4 O2 1.753(11) . ?
W4 O8 1.889(8) . ?
W4 O11 1.952(7) . ?
W4 O18 1.981(10) . ?
W4 O14 2.414(6) . ?
W5 O21 1.729(11) . ?
W5 O15 1.865(9) . ?
W5 O20 1.855(8) 3_655 ?
W5 O19 1.883(9) . ?
W5 O16 2.063(10) . ?
W5 O13 2.350(9) . ?
W6 O22 1.682(9) . ?
W6 O18 1.868(9) . ?
W6 O19 1.889(9) . ?
W6 O20 1.959(8) . ?
W6 O17 2.006(7) . ?
W6 O14 2.233(7) . ?
Cu1 O2 1.916(8) . ?
Cu1 O1 1.935(9) . ?
Cu1 O3 2.025(8) 3_655 ?
Cu1 O3 2.031(8) . ?
Cu1 O101 2.105(9) . ?
Cu1 Cu1 2.892(2) 3_655 ?
O3 P1 1.532(7) 3_655 ?
O3 Cu1 2.025(8) 3_655 ?
O9 W2 1.809(9) 3_655 ?
O13 P1 1.497(7) 3_655 ?
O16 W2 1.779(12) 3_655 ?
O20 W5 1.855(8) 3_655 ?
O101 C101 1.237(12) . ?
C101 O101 1.237(12) 3_655 ?
C101 C102 1.462(10) . ?
C102 H10A 0.9600 . ?
C102 H10B 0.9600 . ?
C102 H10C 0.9600 . ?
O201 C201 1.24(2) . ?
N201 C201 1.45(2) . ?
N1 C141 1.44(3) . ?
N1 C131 1.56(3) . ?
N1 C121 1.52(3) . ?
N1 C111 1.65(3) . ?
C111 C112 1.5501(10) . ?
C112 C113 1.64(3) . ?
C113 C114 1.5500(10) . ?
C121 C122 1.60(3) . ?
C122 C123 1.71(3) . ?
C123 C124 1.35(3) . ?
C131 C132 1.64(3) . ?
C132 C133 1.56(3) . ?
C133 C134 1.5499(10) . ?
C141 C142 1.43(3) . ?
C142 C143 1.5497(10) . ?
C143 C144 1.5499(10) . ?
N2 C211 1.45(2) . ?
N2 C211 1.45(2) 3_655 ?
N2 C221 1.42(2) 3_655 ?
N2 C221 1.42(2) . ?
C201 C202 1.44(2) . ?
C202 H20A 0.9600 . ?
C202 H20B 0.9600 . ?
C202 H20C 0.9600 . ?
C211 C212 1.66(2) . ?
C212 C213 1.62(2) . ?
C213 C214 1.5500(10) . ?
C221 C222 1.5497(10) . ?
C222 C223 1.5500(10) . ?
C223 C224 1.5501(10) . ?

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
O13 P1 O3 105.5(5) 3_655 3_655 ?
O13 P1 O12 108.4(4) 3_655 . ?
O3 P1 O12 112.2(4) 3_655 . ?
O13 P1 O14 113.2(3) 3_655 . ?
O3 P1 O14 110.6(4) 3_655 . ?
O12 P1 O14 107.1(4) . . ?
O4 W1 O1 103.4(4) . . ?
O4 W1 O8 100.6(4) . . ?
O1 W1 O8 92.6(3) . . ?
O4 W1 O15 104.0(4) . . ?
O1 W1 O15 152.6(3) . . ?
O8 W1 O15 81.2(3) . . ?
O4 W1 O9 95.3(4) . . ?
O1 W1 O9 92.9(4) . . ?
O8 W1 O9 161.5(4) . . ?
O15 W1 O9 85.8(5) . . ?
O4 W1 O13 171.4(4) . . ?
O1 W1 O13 82.2(3) . . ?
O8 W1 O13 85.5(3) . . ?
O15 W1 O13 70.7(3) . . ?
O9 W1 O13 77.8(3) . . ?
O16 W2 O5 101.8(4) 3_655 . ?
O16 W2 O9 96.1(5) 3_655 3_655 ?
O5 W2 O9 102.2(4) . 3_655 ?
O16 W2 O10 92.6(3) 3_655 . ?
O5 W2 O10 98.8(4) . . ?
O9 W2 O10 155.0(4) 3_655 . ?
O16 W2 O201 161.1(3) 3_655 . ?
O5 W2 O201 96.0(4) . . ?
O9 W2 O201 86.2(5) 3_655 . ?
O10 W2 O201 78.3(4) . . ?
O16 W2 O12 87.4(3) 3_655 . ?
O5 W2 O12 168.4(3) . . ?
O9 W2 O12 83.7(3) 3_655 . ?
O10 W2 O12 73.4(3) . . ?
O201 W2 O12 74.2(3) . . ?
O6 W3 O17 106.4(7) . . ?
O6 W3 O11 98.9(5) . . ?
O17 W3 O11 92.0(4) . . ?
O6 W3 O10 98.9(5) . . ?
O17 W3 O10 94.2(4) . . ?
O11 W3 O10 158.6(4) . . ?
O6 W3 N201 88.6(7) . . ?
O17 W3 N201 165.0(4) . . ?
O11 W3 N201 86.7(4) . . ?
O10 W3 N201 82.1(4) . . ?
O6 W3 O12 165.3(5) . . ?
O17 W3 O12 87.3(3) . . ?
O11 W3 O12 85.5(3) . . ?
O10 W3 O12 74.3(3) . . ?
N201 W3 O12 77.6(3) . . ?
O7 W4 O2 109.3(5) . . ?
O7 W4 O8 98.5(3) . . ?
O2 W4 O8 90.4(4) . . ?
O7 W4 O11 94.8(3) . . ?
O2 W4 O11 97.2(4) . . ?
O8 W4 O11 161.6(3) . . ?
O7 W4 O18 98.6(5) . . ?
O2 W4 O18 152.0(4) . . ?
O8 W4 O18 82.2(3) . . ?
O11 W4 O18 83.3(4) . . ?
O7 W4 O14 165.9(5) . . ?
O2 W4 O14 84.3(3) . . ?
O8 W4 O14 84.7(3) . . ?
O11 W4 O14 79.4(3) . . ?
O18 W4 O14 68.2(3) . . ?
O21 W5 O15 100.1(5) . . ?
O21 W5 O20 101.6(4) . 3_655 ?
O15 W5 O20 156.7(4) . 3_655 ?
O21 W5 O19 99.0(3) . . ?
O15 W5 O19 93.5(3) . . ?
O20 W5 O19 91.3(3) 3_655 . ?
O21 W5 O16 94.4(4) . . ?
O15 W5 O16 82.9(4) . . ?
O20 W5 O16 87.0(3) 3_655 . ?
O19 W5 O16 166.5(3) . . ?
O21 W5 O13 173.5(4) . . ?
O15 W5 O13 74.1(4) . . ?
O20 W5 O13 83.7(3) 3_655 . ?
O19 W5 O13 84.4(2) . . ?
O16 W5 O13 82.1(3) . . ?
O22 W6 O18 102.7(5) . . ?
O22 W6 O19 98.7(4) . . ?
O18 W6 O19 94.6(3) . . ?
O22 W6 O20 100.8(4) . . ?
O18 W6 O20 154.9(3) . . ?
O19 W6 O20 90.5(2) . . ?
O22 W6 O17 95.7(5) . . ?
O18 W6 O17 83.0(4) . . ?
O19 W6 O17 165.5(4) . . ?
O20 W6 O17 85.9(3) . . ?
O22 W6 O14 176.5(4) . . ?
O18 W6 O14 74.1(3) . . ?
O19 W6 O14 83.2(2) . . ?
O20 W6 O14 82.1(3) . . ?
O17 W6 O14 82.4(4) . . ?
O2 Cu1 O1 89.8(3) . . ?
O2 Cu1 O3 91.2(3) . 3_655 ?
O1 Cu1 O3 160.6(3) . 3_655 ?
O2 Cu1 O3 158.5(4) . . ?
O1 Cu1 O3 89.4(3) . . ?
O3 Cu1 O3 82.7(3) 3_655 . ?
O2 Cu1 O101 102.3(5) . . ?
O1 Cu1 O101 104.1(5) . . ?
O3 Cu1 O101 94.7(4) 3_655 . ?
O3 Cu1 O101 98.7(4) . . ?
O2 Cu1 Cu1 135.5(3) . 3_655 ?
O1 Cu1 Cu1 133.2(3) . 3_655 ?
O3 Cu1 Cu1 44.6(2) 3_655 3_655 ?
O3 Cu1 Cu1 44.5(2) . 3_655 ?
O101 Cu1 Cu1 80.7(3) . 3_655 ?
W1 O1 Cu1 122.4(4) . . ?
W4 O2 Cu1 126.7(6) . . ?
P1 O3 Cu1 117.4(4) 3_655 3_655 ?
P1 O3 Cu1 118.6(5) 3_655 . ?
Cu1 O3 Cu1 90.9(3) 3_655 . ?
W4 O8 W1 146.9(4) . . ?
W2 O9 W1 141.2(7) 3_655 . ?
W3 O10 W2 119.0(3) . . ?
W3 O11 W4 143.4(4) . . ?
P1 O12 W3 126.4(4) . . ?
P1 O12 W2 125.8(4) . . ?
W3 O12 W2 93.2(2) . . ?
P1 O13 W5 124.7(5) 3_655 . ?
P1 O13 W1 128.0(5) 3_655 . ?
W5 O13 W1 91.7(2) . . ?
P1 O14 W6 129.2(4) . . ?
P1 O14 W4 122.1(4) . . ?
W6 O14 W4 93.8(2) . . ?
W5 O15 W1 123.3(4) . . ?
W2 O16 W5 140.1(5) 3_655 . ?
W3 O17 W6 141.2(6) . . ?
W6 O18 W4 123.8(4) . . ?
W6 O19 W5 171.0(3) . . ?
W5 O20 W6 162.7(4) 3_655 . ?
C101 O101 Cu1 124.9(10) . . ?
O101 C101 O101 127.9(18) . 3_655 ?
O101 C101 C102 116.1(9) . . ?
O101 C101 C102 116.1(9) 3_655 . ?
C101 C102 H10A 109.5 . . ?
C101 C102 H10B 109.5 . . ?
H10A C102 H10B 109.5 . . ?
C101 C102 H10C 109.5 . . ?
H10A C102 H10C 109.5 . . ?
H10B C102 H10C 109.5 . . ?
C201 O201 W2 137.3(11) . . ?
C201 N201 W3 126.9(10) . . ?
C141 N1 C131 95(2) . . ?
C141 N1 C121 115.1(19) . . ?
C131 N1 C121 101.8(18) . . ?
C141 N1 C111 108.1(17) . . ?
C131 N1 C111 120.8(18) . . ?
C121 N1 C111 114.8(18) . . ?
C112 C111 N1 109.8(15) . . ?
C111 C112 C113 103.8(16) . . ?
C114 C113 C112 106.0(14) . . ?
N1 C121 C122 108.4(17) . . ?
C121 C122 C123 102.0(16) . . ?
C124 C123 C122 114(2) . . ?
N1 C131 C132 109(2) . . ?
C133 C132 C131 110(2) . . ?
C132 C133 C134 110.3(15) . . ?
N1 C141 C142 117(2) . . ?
C141 C142 C143 117.7(16) . . ?
C142 C143 C144 111.0(3) . . ?
C211 N2 C211 108(2) . 3_655 ?
C211 N2 C221 103.4(12) . 3_655 ?
C211 N2 C221 122.4(13) 3_655 3_655 ?
C211 N2 C221 122.4(13) . . ?
C211 N2 C221 103.4(12) 3_655 . ?
C221 N2 C221 98.6(19) 3_655 . ?
O201 C201 N201 121.9(12) . . ?
O201 C201 C202 132(2) . . ?
N201 C201 C202 105.4(18) . . ?
C201 C202 H20A 109.5 . . ?
C201 C202 H20B 109.5 . . ?
H20A C202 H20B 109.5 . . ?
C201 C202 H20C 109.5 . . ?
H20A C202 H20C 109.5 . . ?
H20B C202 H20C 109.5 . . ?
N2 C211 C212 112.9(15) . . ?
C211 C212 C213 109.8(16) . . ?
C214 C213 C212 107.3(12) . . ?
C222 C221 N2 116.9(15) . . ?
C221 C222 C223 111.8(16) . . ?
C224 C223 C222 110.3(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 W1 O1 Cu1 147.7(5) . . . . ?
O8 W1 O1 Cu1 46.2(5) . . . . ?
O15 W1 O1 Cu1 -29.6(10) . . . . ?
O9 W1 O1 Cu1 -116.2(5) . . . . ?
O13 W1 O1 Cu1 -38.9(4) . . . . ?
O7 W4 O2 Cu1 -147.6(5) . . . . ?
O8 W4 O2 Cu1 -48.4(6) . . . . ?
O11 W4 O2 Cu1 114.7(6) . . . . ?
O18 W4 O2 Cu1 25.4(12) . . . . ?
O14 W4 O2 Cu1 36.2(5) . . . . ?
O7 W4 O8 W1 115.7(8) . . . . ?
O2 W4 O8 W1 6.1(7) . . . . ?
O11 W4 O8 W1 -108.5(12) . . . . ?
O18 W4 O8 W1 -146.8(7) . . . . ?
O14 W4 O8 W1 -78.1(7) . . . . ?
O6 W3 O11 W4 -129.0(10) . . . . ?
O17 W3 O11 W4 -22.1(9) . . . . ?
O10 W3 O11 W4 84.6(13) . . . . ?
N201 W3 O11 W4 142.9(9) . . . . ?
O12 W3 O11 W4 65.1(8) . . . . ?
O13 P1 O12 W3 -126.9(5) 3_655 . . . ?
O3 P1 O12 W3 117.1(5) 3_655 . . . ?
O14 P1 O12 W3 -4.4(6) . . . . ?
O13 P1 O12 W2 1.2(6) 3_655 . . . ?
O3 P1 O12 W2 -114.8(5) 3_655 . . . ?
O14 P1 O12 W2 123.7(5) . . . . ?
O13 P1 O14 W6 59.3(6) 3_655 . . . ?
O3 P1 O14 W6 177.4(4) 3_655 . . . ?
O12 P1 O14 W6 -60.1(6) . . . . ?
O13 P1 O14 W4 -172.9(5) 3_655 . . . ?
O3 P1 O14 W4 -54.8(5) 3_655 . . . ?
O12 P1 O14 W4 67.7(5) . . . . ?
O21 W5 O15 W1 -174.0(5) . . . . ?
O20 W5 O15 W1 -15.4(11) 3_655 . . . ?
O19 W5 O15 W1 86.2(5) . . . . ?
O16 W5 O15 W1 -80.7(5) . . . . ?
O13 W5 O15 W1 3.0(4) . . . . ?
O6 W3 O17 W6 127.2(8) . . . . ?
O11 W3 O17 W6 27.3(8) . . . . ?
O10 W3 O17 W6 -132.2(7) . . . . ?
N201 W3 O17 W6 -57.2(19) . . . . ?
O12 W3 O17 W6 -58.1(7) . . . . ?
O22 W6 O18 W4 175.8(5) . . . . ?
O19 W6 O18 W4 -84.2(5) . . . . ?
O20 W6 O18 W4 16.9(11) . . . . ?
O17 W6 O18 W4 81.5(6) . . . . ?
O14 W6 O18 W4 -2.6(4) . . . . ?
Cu1 O101 C101 O101 -4.9(6) . . . 3_655 ?
Cu1 O101 C101 C102 175.1(6) . . . . ?
C141 N1 C111 C112 176(2) . . . . ?
C131 N1 C111 C112 68(3) . . . . ?
C121 N1 C111 C112 -54(2) . . . . ?
N1 C111 C112 C113 172.3(16) . . . . ?
C111 C112 C113 C114 120.5(18) . . . . ?
C141 N1 C121 C122 61(3) . . . . ?
C131 N1 C121 C122 162(2) . . . . ?
C111 N1 C121 C122 -65(2) . . . . ?
N1 C121 C122 C123 -178.4(17) . . . . ?
C121 C122 C123 C124 -63(3) . . . . ?
C141 N1 C131 C132 -76(2) . . . . ?
C121 N1 C131 C132 166.7(18) . . . . ?
C111 N1 C131 C132 38(3) . . . . ?
N1 C131 C132 C133 -165.1(19) . . . . ?
C131 C132 C133 C134 70(3) . . . . ?
C131 N1 C141 C142 -50(3) . . . . ?
C121 N1 C141 C142 56(3) . . . . ?
C111 N1 C141 C142 -174(2) . . . . ?
N1 C141 C142 C143 -171(2) . . . . ?
C141 C142 C143 C144 -174(3) . . . . ?
W2 O201 C201 N201 1(2) . . . . ?
W2 O201 C201 C202 168.2(14) . . . . ?
W3 N201 C201 O201 -1(2) . . . . ?
W3 N201 C201 C202 -171.4(11) . . . . ?
C211 N2 C211 C212 156(2) 3_655 . . . ?
C221 N2 C211 C212 -73.1(19) 3_655 . . . ?
C221 N2 C211 C212 36(2) . . . . ?
N2 C211 C212 C213 160.1(14) . . . . ?
C211 C212 C213 C214 175.8(17) . . . . ?
C211 N2 C221 C222 63(3) . . . . ?
C211 N2 C221 C222 -59(2) 3_655 . . . ?
C221 N2 C221 C222 175(3) 3_655 . . . ?
N2 C221 C222 C223 -176.4(19) . . . . ?
C221 C222 C223 C224 131(2) . . . . ?

_refine_diff_density_max         1.699
_refine_diff_density_min         -2.526
_refine_diff_density_rms         0.494

_shelxl_version_number           2014/6




loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.122 -0.002 0.001 5652 5617 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ni2
_database_code_depnum_ccdc_archive 'CCDC 1883424'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H9 N5 Ni2 O48 P2 W12'
_chemical_formula_weight         3881.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
W W -0.8490 6.8722 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_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, -z'
'-x, y, -z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'

_cell_length_a                   19.0988(2)
_cell_length_b                   28.2884(4)
_cell_length_c                   24.8669(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13435.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9850
_cell_measurement_theta_min      1.286
_cell_measurement_theta_max      29.450

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_F_000             6972
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    10.584
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9925
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.286
_diffrn_reflns_theta_max         29.450
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.532
_diffrn_reflns_point_group_measured_fraction_full 0.538
_reflns_number_total             9925
_reflns_number_gt                8089
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.000
_reflns_Friedel_fraction_full    0.000

_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       'Rigaku CrystalClear'
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1269P)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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.02(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9925
_refine_ls_number_parameters     397
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1801
_refine_ls_wR_factor_gt          0.1723
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_restrained_S_all      1.150
_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
W1 W -0.09636(3) 0.36026(3) 0.39152(2) 0.0447(2) Uani 1 1 d . . . . .
W2 W -0.25251(3) 0.32822(4) 0.31580(3) 0.0540(2) Uani 1 1 d . . . . .
W3 W 0.25209(3) 0.32836(3) 0.31740(3) 0.0488(2) Uani 1 1 d . . . . .
W4 W 0.09449(3) 0.36077(3) 0.39212(2) 0.0440(2) Uani 1 1 d . . . . .
W5 W 0.09850(3) 0.25518(3) 0.17452(3) 0.04010(17) Uani 1 1 d . U . . .
W6 W 0.09813(3) 0.25504(2) 0.32606(2) 0.03827(16) Uani 1 1 d . U . . .
Ni1 Ni -0.00081(13) 0.42382(4) 0.30816(5) 0.0405(3) Uani 1 1 d . . . . .
P1 P 0.10093(11) 0.35715(8) 0.25151(16) 0.0294(4) Uani 1 1 d . . . . .
O1 O -0.0724(5) 0.4155(5) 0.3638(4) 0.051(3) Uani 1 1 d . . . . .
O2 O 0.0727(5) 0.4160(4) 0.3637(4) 0.049(3) Uani 1 1 d . . . . .
O3 O 0.0718(4) 0.4072(3) 0.2520(5) 0.0417(16) Uani 1 1 d . . . . .
O4 O -0.1190(5) 0.3726(5) 0.4557(4) 0.056(3) Uani 1 1 d . . . . .
O5 O -0.3211(6) 0.3184(7) 0.3602(5) 0.088(5) Uani 1 1 d . . . . .
O6 O 0.3184(5) 0.3124(6) 0.3597(4) 0.065(4) Uani 1 1 d . . . . .
O7 O 0.1189(6) 0.3734(7) 0.4587(4) 0.086(6) Uani 1 1 d . . . . .
O8 O 0.0031(5) 0.3450(3) 0.4025(3) 0.0449(18) Uani 1 1 d . . . . .
O9 O -0.1932(5) 0.3632(6) 0.3581(5) 0.058(3) Uani 1 1 d . . . . .
O10 O 0.2971(3) 0.3126(3) 0.2552(5) 0.051(2) Uani 1 1 d . . . . .
O11 O 0.1905(4) 0.3595(5) 0.3636(3) 0.039(2) Uani 1 1 d . . . . .
O12 O 0.1819(3) 0.3573(2) 0.2488(5) 0.0414(15) Uani 1 1 d . . . . .
O13 O 0.0765(5) 0.3343(4) 0.1981(3) 0.040(3) Uani 1 1 d . . . . .
O14 O 0.0758(4) 0.3297(4) 0.3012(3) 0.0247(17) Uani 1 1 d . . . . .
O15 O -0.1013(5) 0.2900(5) 0.3896(4) 0.048(3) Uani 1 1 d . . . . .
O16 O 0.1986(4) 0.2735(4) 0.1860(4) 0.034(2) Uani 1 1 d . . . . .
O17 O 0.2000(5) 0.2802(6) 0.3165(4) 0.063(4) Uani 1 1 d . . . . .
O18 O 0.1084(4) 0.2909(5) 0.3880(4) 0.045(3) Uani 1 1 d . . . . .
O19 O -0.0003(5) 0.2512(2) 0.1716(3) 0.0377(15) Uani 1 1 d . . . . .
O20 O 0.0974(3) 0.2460(2) 0.2518(5) 0.0373(14) Uani 1 1 d . U . . .
O21 O 0.1172(5) 0.1966(4) 0.1526(5) 0.057(3) Uani 1 1 d . . . . .
O22 O 0.1179(5) 0.2033(5) 0.3484(4) 0.053(3) Uani 1 1 d . U . . .
C201 C 0.3124(9) 0.4142(5) 0.2562(10) 0.070(4) Uiso 1 1 d . U . . .
C202 C 0.3524(15) 0.4610(7) 0.2526(15) 0.123(7) Uiso 1 1 d . U . . .
H20A H 0.3520 0.4720 0.2161 0.185 Uiso 1 1 calc R U . . .
H20B H 0.3304 0.4840 0.2754 0.185 Uiso 1 1 calc R U . . .
H20C H 0.3999 0.4562 0.2640 0.185 Uiso 1 1 calc R U . . .
O201 O 0.2950(6) 0.4005(4) 0.2046(5) 0.060(3) Uiso 1 1 d . U . . .
N201 N 0.3013(8) 0.3883(5) 0.2984(6) 0.059(3) Uiso 1 1 d . U . . .
C101 C 0.0000 0.5111(6) 0.2500 0.078(5) Uiso 1 2 d DS U P . .
C102 C 0.0000 0.5658(6) 0.2500 0.123(10) Uiso 1 2 d DS U P . .
H10A H 0.0072 0.5772 0.2860 0.184 Uiso 0.5 1 calc R U P . .
H10B H 0.0369 0.5772 0.2272 0.184 Uiso 0.5 1 calc R U P . .
H10C H -0.0442 0.5772 0.2368 0.184 Uiso 0.5 1 calc R U P . .
O101 O 0.0091(7) 0.4926(3) 0.2950(4) 0.061(2) Uiso 1 1 d . U . . .
N1 N 0.7838(10) 0.2084(5) 0.4944(10) 0.146(5) Uiso 1 1 d D U . . .
C111 C 0.8600(9) 0.2227(9) 0.4803(9) 0.102(5) Uiso 1 1 d D U . . .
C112 C 0.9055(9) 0.2221(9) 0.5258(10) 0.101(6) Uiso 1 1 d D U . . .
C113 C 0.9762(10) 0.2467(9) 0.5136(11) 0.118(7) Uiso 1 1 d D U . . .
C114 C 1.0089(16) 0.2163(13) 0.4905(15) 0.172(11) Uiso 1 1 d . U . . .
C121 C 0.7476(17) 0.2468(6) 0.5256(11) 0.136(7) Uiso 1 1 d D U . . .
C122 C 0.7308(18) 0.2931(8) 0.5070(10) 0.139(7) Uiso 1 1 d D U . . .
C123 C 0.7253(19) 0.3333(6) 0.5492(10) 0.143(8) Uiso 1 1 d D U . . .
C124 C 0.7028(17) 0.3808(8) 0.5174(13) 0.149(10) Uiso 1 1 d D U . . .
C131 C 0.7806(17) 0.1596(5) 0.5226(8) 0.165(8) Uiso 1 1 d D U . . .
C132 C 0.7549(18) 0.1209(5) 0.4832(11) 0.210(10) Uiso 1 1 d D U . . .
C133 C 0.7920(14) 0.0816(8) 0.5160(14) 0.208(11) Uiso 1 1 d D U . . .
C134 C 0.7507(19) 0.0345(7) 0.512(2) 0.225(13) Uiso 1 1 d D U . . .
C141 C 0.7441(11) 0.2105(12) 0.4318(11) 0.152(7) Uiso 1 1 d D U . . .
C142 C 0.6663(11) 0.1957(12) 0.4376(9) 0.168(8) Uiso 1 1 d D U . . .
C143 C 0.6281(15) 0.2051(13) 0.3837(8) 0.167(9) Uiso 1 1 d D U . . .
C144 C 0.5877(17) 0.1989(18) 0.3300(10) 0.193(15) Uiso 1 1 d D U . . .
N2 N 0.0000 0.0950(8) 0.2500 0.093(5) Uiso 1 2 d S U P . .
C211 C 0.0595(10) 0.1268(7) 0.2492(11) 0.088(4) Uiso 1 1 d . U . . .
C212 C 0.1317(11) 0.0988(7) 0.2630(9) 0.089(5) Uiso 1 1 d . U . . .
C213 C 0.1972(11) 0.1327(7) 0.2585(10) 0.088(5) Uiso 1 1 d . U . . .
C214 C 0.2664(14) 0.1035(9) 0.2374(12) 0.114(8) Uiso 1 1 d . U . . .
C221 C 0.0108(14) 0.0630(8) 0.2987(6) 0.100(5) Uiso 1 1 d D U . . .
C222 C -0.0069(16) 0.0866(7) 0.3479(6) 0.123(6) Uiso 1 1 d D U . . .
C223 C -0.0244(18) 0.0551(7) 0.3971(7) 0.159(9) Uiso 1 1 d D U . . .
C224 C -0.036(3) 0.0857(11) 0.4481(7) 0.239(16) Uiso 1 1 d D U . . .


_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
W1 O4 1.691(10) . ?
W1 O1 1.768(14) . ?
W1 O8 1.967(9) . ?
W1 O15 1.991(13) . ?
W1 O9 2.029(11) . ?
W1 O13 2.377(9) 3 ?
W2 O5 1.735(13) . ?
W2 O9 1.836(14) . ?
W2 O16 1.861(10) 3 ?
W2 O10 2.009(11) 3 ?
W2 O12 2.253(10) 3 ?
W2 O201 2.258(13) 3 ?
W3 O17 1.687(15) . ?
W3 O6 1.706(9) . ?
W3 O10 1.825(11) . ?
W3 O11 1.865(10) . ?
W3 N201 1.995(15) . ?
W3 O12 2.319(10) . ?
W4 O7 1.757(10) . ?
W4 O2 1.764(12) . ?
W4 O8 1.820(10) . ?
W4 O11 1.967(8) . ?
W4 O18 1.997(13) . ?
W4 O14 2.451(8) . ?
W5 O21 1.781(11) . ?
W5 O15 1.874(11) 3 ?
W5 O19 1.892(9) . ?
W5 O20 1.939(12) . ?
W5 O16 2.001(9) . ?
W5 O13 2.353(12) . ?
W6 O22 1.611(12) . ?
W6 O18 1.855(11) . ?
W6 O20 1.865(12) . ?
W6 O19 1.872(10) 3 ?
W6 O17 2.086(11) . ?
W6 O14 2.242(10) . ?
Ni1 O1 1.959(10) . ?
Ni1 O101 1.981(9) . ?
Ni1 O2 1.982(11) . ?
Ni1 O3 2.024(10) . ?
Ni1 O3 2.074(11) 3 ?
Ni1 Ni1 2.893(3) 3 ?
P1 O3 1.521(8) . ?
P1 O14 1.536(9) . ?
P1 O13 1.548(10) . ?
P1 O12 1.548(7) . ?
O3 Ni1 2.074(11) 3 ?
O10 W2 2.010(11) 3 ?
O12 W2 2.253(10) 3 ?
O13 W1 2.377(9) 3 ?
O15 W5 1.874(11) 3 ?
O16 W2 1.860(10) 3 ?
O19 W6 1.872(9) 3 ?
C201 N201 1.30(2) . ?
C201 O201 1.38(2) . ?
C201 C202 1.53(2) . ?
C202 H20A 0.9600 . ?
C202 H20B 0.9600 . ?
C202 H20C 0.9600 . ?
O201 W2 2.258(13) 3 ?
C101 O101 1.248(11) 3 ?
C101 O101 1.248(11) . ?
C101 C102 1.5500(10) . ?
C102 H10A 0.9600 . ?
C102 H10B 0.9600 . ?
C102 H10C 0.9600 . ?
N1 C121 1.51(2) . ?
N1 C111 1.5500(10) . ?
N1 C131 1.5500(10) . ?
N1 C141 1.73(4) . ?
C111 C112 1.43(3) . ?
C112 C113 1.5500(10) . ?
C113 C114 1.21(4) . ?
C121 C122 1.43(3) . ?
C122 C123 1.5500(10) . ?
C123 C124 1.62(3) . ?
C131 C132 1.5500(10) . ?
C132 C133 1.5501(10) . ?
C133 C134 1.5500(10) . ?
C134 C134 2.05(6) 2_556 ?
C141 C142 1.5500(10) . ?
C142 C143 1.5500(10) . ?
C143 C144 1.5500(10) . ?
N2 C211 1.45(2) . ?
N2 C211 1.45(2) 3 ?
N2 C221 1.53(2) . ?
N2 C221 1.53(2) 3 ?
C211 C212 1.63(3) . ?
C212 C213 1.58(3) . ?
C213 C214 1.65(3) . ?
C221 C222 1.43(2) . ?
C222 C223 1.5501(10) . ?
C223 C224 1.5500(10) . ?

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
O4 W1 O1 104.6(5) . . ?
O4 W1 O8 99.3(4) . . ?
O1 W1 O8 89.9(4) . . ?
O4 W1 O15 102.5(6) . . ?
O1 W1 O15 152.3(4) . . ?
O8 W1 O15 80.2(4) . . ?
O4 W1 O9 98.3(5) . . ?
O1 W1 O9 92.3(5) . . ?
O8 W1 O9 161.1(4) . . ?
O15 W1 O9 89.3(6) . . ?
O4 W1 O13 171.9(5) . 3 ?
O1 W1 O13 82.3(4) . 3 ?
O8 W1 O13 84.7(3) . 3 ?
O15 W1 O13 71.1(4) . 3 ?
O9 W1 O13 76.9(4) . 3 ?
O5 W2 O9 100.8(6) . . ?
O5 W2 O16 107.4(7) . 3 ?
O9 W2 O16 96.9(5) . 3 ?
O5 W2 O10 101.8(5) . 3 ?
O9 W2 O10 152.1(5) . 3 ?
O16 W2 O10 91.8(4) 3 3 ?
O5 W2 O12 164.5(6) . 3 ?
O9 W2 O12 80.9(4) . 3 ?
O16 W2 O12 87.5(3) 3 3 ?
O10 W2 O12 73.0(4) 3 3 ?
O5 W2 O201 90.9(7) . 3 ?
O9 W2 O201 82.1(5) . 3 ?
O16 W2 O201 161.4(4) 3 3 ?
O10 W2 O201 81.3(4) 3 3 ?
O12 W2 O201 74.0(3) 3 3 ?
O17 W3 O6 103.5(7) . . ?
O17 W3 O10 93.9(5) . . ?
O6 W3 O10 96.2(5) . . ?
O17 W3 O11 91.0(5) . . ?
O6 W3 O11 102.3(6) . . ?
O10 W3 O11 159.2(4) . . ?
O17 W3 N201 163.9(6) . . ?
O6 W3 N201 91.2(6) . . ?
O10 W3 N201 77.6(5) . . ?
O11 W3 N201 92.4(6) . . ?
O17 W3 O12 86.2(4) . . ?
O6 W3 O12 167.3(4) . . ?
O10 W3 O12 74.7(4) . . ?
O11 W3 O12 85.5(4) . . ?
N201 W3 O12 78.4(4) . . ?
O7 W4 O2 105.0(7) . . ?
O7 W4 O8 99.8(5) . . ?
O2 W4 O8 92.7(4) . . ?
O7 W4 O11 95.5(4) . . ?
O2 W4 O11 95.3(5) . . ?
O8 W4 O11 160.2(4) . . ?
O7 W4 O18 102.4(7) . . ?
O2 W4 O18 152.5(5) . . ?
O8 W4 O18 83.9(3) . . ?
O11 W4 O18 80.7(5) . . ?
O7 W4 O14 168.7(6) . . ?
O2 W4 O14 85.0(4) . . ?
O8 W4 O14 84.5(3) . . ?
O11 W4 O14 78.3(3) . . ?
O18 W4 O14 67.5(4) . . ?
O21 W5 O15 102.8(6) . 3 ?
O21 W5 O19 97.6(4) . . ?
O15 W5 O19 91.6(4) 3 . ?
O21 W5 O20 100.4(5) . . ?
O15 W5 O20 156.0(4) 3 . ?
O19 W5 O20 91.1(3) . . ?
O21 W5 O16 95.3(4) . . ?
O15 W5 O16 87.6(4) 3 . ?
O19 W5 O16 166.9(3) . . ?
O20 W5 O16 84.5(3) . . ?
O21 W5 O13 176.3(5) . . ?
O15 W5 O13 73.6(4) 3 . ?
O19 W5 O13 83.6(3) . . ?
O20 W5 O13 83.0(3) . . ?
O16 W5 O13 83.6(4) . . ?
O22 W6 O18 100.7(5) . . ?
O22 W6 O20 102.7(5) . . ?
O18 W6 O20 153.9(4) . . ?
O22 W6 O19 99.8(4) . 3 ?
O18 W6 O19 96.5(3) . 3 ?
O20 W6 O19 90.8(3) . 3 ?
O22 W6 O17 97.5(6) . . ?
O18 W6 O17 79.0(4) . . ?
O20 W6 O17 86.6(3) . . ?
O19 W6 O17 162.6(5) 3 . ?
O22 W6 O14 174.9(5) . . ?
O18 W6 O14 74.6(4) . . ?
O20 W6 O14 81.6(3) . . ?
O19 W6 O14 82.7(3) 3 . ?
O17 W6 O14 79.9(5) . . ?
O1 Ni1 O101 107.5(5) . . ?
O1 Ni1 O2 89.3(3) . . ?
O101 Ni1 O2 99.1(5) . . ?
O1 Ni1 O3 159.7(4) . . ?
O101 Ni1 O3 92.8(4) . . ?
O2 Ni1 O3 88.2(4) . . ?
O1 Ni1 O3 91.5(4) . 3 ?
O101 Ni1 O3 99.5(4) . 3 ?
O2 Ni1 O3 160.2(4) . 3 ?
O3 Ni1 O3 84.2(3) . 3 ?
O1 Ni1 Ni1 135.5(3) . 3 ?
O101 Ni1 Ni1 80.5(3) . 3 ?
O2 Ni1 Ni1 133.6(3) . 3 ?
O3 Ni1 Ni1 45.8(3) . 3 ?
O3 Ni1 Ni1 44.4(3) 3 3 ?
O3 P1 O14 110.4(6) . . ?
O3 P1 O13 106.6(7) . . ?
O14 P1 O13 112.7(4) . . ?
O3 P1 O12 111.3(4) . . ?
O14 P1 O12 110.4(5) . . ?
O13 P1 O12 105.4(6) . . ?
W1 O1 Ni1 124.2(6) . . ?
W4 O2 Ni1 123.1(6) . . ?
P1 O3 Ni1 118.2(5) . . ?
P1 O3 Ni1 116.3(6) . 3 ?
Ni1 O3 Ni1 89.8(3) . 3 ?
W4 O8 W1 148.5(4) . . ?
W2 O9 W1 140.8(8) . . ?
W3 O10 W2 119.4(4) . 3 ?
W3 O11 W4 145.0(6) . . ?
P1 O12 W2 128.9(6) . 3 ?
P1 O12 W3 123.0(6) . . ?
W2 O12 W3 92.8(2) 3 . ?
P1 O13 W5 123.8(6) . . ?
P1 O13 W1 128.9(6) . 3 ?
W5 O13 W1 91.8(3) . 3 ?
P1 O14 W6 129.6(5) . . ?
P1 O14 W4 121.0(5) . . ?
W6 O14 W4 93.2(3) . . ?
W5 O15 W1 122.9(6) 3 . ?
W2 O16 W5 137.8(5) 3 . ?
W3 O17 W6 145.5(8) . . ?
W6 O18 W4 124.7(5) . . ?
W6 O19 W5 172.2(4) 3 . ?
W6 O20 W5 164.4(4) . . ?
N201 C201 O201 123.6(14) . . ?
N201 C201 C202 128(2) . . ?
O201 C201 C202 108(2) . . ?
C201 C202 H20A 109.5 . . ?
C201 C202 H20B 109.5 . . ?
H20A C202 H20B 109.5 . . ?
C201 C202 H20C 109.5 . . ?
H20A C202 H20C 109.5 . . ?
H20B C202 H20C 109.5 . . ?
C201 O201 W2 123.4(10) . 3 ?
C201 N201 W3 138.5(12) . . ?
O101 C101 O101 130.5(16) 3 . ?
O101 C101 C102 114.8(8) 3 . ?
O101 C101 C102 114.8(8) . . ?
C101 C102 H10A 109.5 . . ?
C101 C102 H10B 109.5 . . ?
H10A C102 H10B 109.5 . . ?
C101 C102 H10C 109.5 . . ?
H10A C102 H10C 109.5 . . ?
H10B C102 H10C 109.5 . . ?
C101 O101 Ni1 123.1(9) . . ?
C121 N1 C111 111.1(19) . . ?
C121 N1 C131 113.1(14) . . ?
C111 N1 C131 112(2) . . ?
C121 N1 C141 103.7(15) . . ?
C111 N1 C141 101.5(17) . . ?
C131 N1 C141 114.9(15) . . ?
C112 C111 N1 112.9(18) . . ?
C111 C112 C113 111.7(19) . . ?
C114 C113 C112 103(2) . . ?
C122 C121 N1 127(2) . . ?
C121 C122 C123 117.9(18) . . ?
C122 C123 C124 107.2(17) . . ?
C132 C131 N1 110.8(3) . . ?
C131 C132 C133 91.6(15) . . ?
C134 C133 C132 110.7(3) . . ?
C133 C134 C134 147(3) . 2_556 ?
C142 C141 N1 109.1(18) . . ?
C141 C142 C143 109(2) . . ?
C144 C143 C142 164(4) . . ?
C211 N2 C211 103(2) . 3 ?
C211 N2 C221 105.8(13) . . ?
C211 N2 C221 117.7(13) 3 . ?
C211 N2 C221 117.6(13) . 3 ?
C211 N2 C221 105.8(13) 3 3 ?
C221 N2 C221 107(2) . 3 ?
N2 C211 C212 111.0(16) . . ?
C213 C212 C211 111.1(17) . . ?
C212 C213 C214 110.7(17) . . ?
C222 C221 N2 111.7(18) . . ?
C221 C222 C223 117.2(14) . . ?
C224 C223 C222 110.7(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 W1 O1 Ni1 148.0(6) . . . . ?
O8 W1 O1 Ni1 48.5(6) . . . . ?
O15 W1 O1 Ni1 -19.8(13) . . . . ?
O9 W1 O1 Ni1 -112.7(7) . . . . ?
O13 W1 O1 Ni1 -36.2(6) 3 . . . ?
O7 W4 O2 Ni1 -147.2(6) . . . . ?
O8 W4 O2 Ni1 -46.3(6) . . . . ?
O11 W4 O2 Ni1 115.7(6) . . . . ?
O18 W4 O2 Ni1 35.6(12) . . . . ?
O14 W4 O2 Ni1 37.9(6) . . . . ?
O14 P1 O3 Ni1 -8.4(8) . . . . ?
O13 P1 O3 Ni1 114.3(7) . . . . ?
O12 P1 O3 Ni1 -131.4(6) . . . . ?
O14 P1 O3 Ni1 -113.5(6) . . . 3 ?
O13 P1 O3 Ni1 9.1(6) . . . 3 ?
O12 P1 O3 Ni1 123.5(6) . . . 3 ?
O7 W4 O8 W1 112.5(10) . . . . ?
O2 W4 O8 W1 6.7(9) . . . . ?
O11 W4 O8 W1 -107.1(13) . . . . ?
O18 W4 O8 W1 -145.9(8) . . . . ?
O14 W4 O8 W1 -78.0(8) . . . . ?
O5 W2 O9 W1 116.3(11) . . . . ?
O16 W2 O9 W1 7.0(11) 3 . . . ?
O10 W2 O9 W1 -100.2(14) 3 . . . ?
O12 W2 O9 W1 -79.3(10) 3 . . . ?
O201 W2 O9 W1 -154.3(11) 3 . . . ?
O17 W3 O10 W2 82.2(6) . . . 3 ?
O6 W3 O10 W2 -173.8(7) . . . 3 ?
O11 W3 O10 W2 -21.2(15) . . . 3 ?
N201 W3 O10 W2 -83.9(6) . . . 3 ?
O12 W3 O10 W2 -2.8(4) . . . 3 ?
O17 W3 O11 W4 -18.4(12) . . . . ?
O6 W3 O11 W4 -122.4(11) . . . . ?
O10 W3 O11 W4 85.5(18) . . . . ?
N201 W3 O11 W4 145.9(12) . . . . ?
O12 W3 O11 W4 67.7(11) . . . . ?
O3 P1 O12 W2 -117.7(7) . . . 3 ?
O14 P1 O12 W2 119.3(7) . . . 3 ?
O13 P1 O12 W2 -2.6(8) . . . 3 ?
O3 P1 O12 W3 115.5(6) . . . . ?
O14 P1 O12 W3 -7.5(7) . . . . ?
O13 P1 O12 W3 -129.4(6) . . . . ?
O3 P1 O13 W5 -176.4(5) . . . . ?
O14 P1 O13 W5 -55.1(6) . . . . ?
O12 P1 O13 W5 65.3(7) . . . . ?
O3 P1 O13 W1 57.6(8) . . . 3 ?
O14 P1 O13 W1 178.8(7) . . . 3 ?
O12 P1 O13 W1 -60.7(8) . . . 3 ?
O3 P1 O14 W6 -180.0(5) . . . . ?
O13 P1 O14 W6 61.0(7) . . . . ?
O12 P1 O14 W6 -56.5(7) . . . . ?
O3 P1 O14 W4 -54.4(6) . . . . ?
O13 P1 O14 W4 -173.4(6) . . . . ?
O12 P1 O14 W4 69.1(6) . . . . ?
O6 W3 O17 W6 128.1(11) . . . . ?
O10 W3 O17 W6 -134.6(11) . . . . ?
O11 W3 O17 W6 25.2(12) . . . . ?
N201 W3 O17 W6 -77(2) . . . . ?
O12 W3 O17 W6 -60.3(11) . . . . ?
O22 W6 O18 W4 178.7(6) . . . . ?
O20 W6 O18 W4 25.3(10) . . . . ?
O19 W6 O18 W4 -80.1(5) 3 . . . ?
O17 W6 O18 W4 83.0(7) . . . . ?
O14 W6 O18 W4 0.5(5) . . . . ?
O22 W6 O20 W5 -162.2(13) . . . . ?
O18 W6 O20 W5 -9.0(18) . . . . ?
O19 W6 O20 W5 97.6(13) 3 . . . ?
O17 W6 O20 W5 -65.2(14) . . . . ?
O14 W6 O20 W5 15.1(13) . . . . ?
N201 C201 O201 W2 -5(2) . . . 3 ?
C202 C201 O201 W2 168.9(13) . . . 3 ?
O201 C201 N201 W3 -9(3) . . . . ?
C202 C201 N201 W3 178.6(17) . . . . ?
O101 C101 O101 Ni1 -8.2(6) 3 . . . ?
C102 C101 O101 Ni1 171.8(6) . . . . ?
C121 N1 C111 C112 72(3) . . . . ?
C131 N1 C111 C112 -55(2) . . . . ?
C141 N1 C111 C112 -178(2) . . . . ?
N1 C111 C112 C113 -168(2) . . . . ?
C111 C112 C113 C114 -81(3) . . . . ?
C111 N1 C121 C122 65(4) . . . . ?
C131 N1 C121 C122 -168(3) . . . . ?
C141 N1 C121 C122 -43(4) . . . . ?
N1 C121 C122 C123 -153(3) . . . . ?
C121 C122 C123 C124 -178(3) . . . . ?
C121 N1 C131 C132 130(2) . . . . ?
C111 N1 C131 C132 -104(3) . . . . ?
C141 N1 C131 C132 11(3) . . . . ?
N1 C131 C132 C133 155(2) . . . . ?
C131 C132 C133 C134 148(3) . . . . ?
C132 C133 C134 C134 117(5) . . . 2_556 ?
C121 N1 C141 C142 -66(3) . . . . ?
C111 N1 C141 C142 179(2) . . . . ?
C131 N1 C141 C142 58(3) . . . . ?
N1 C141 C142 C143 171(2) . . . . ?
C141 C142 C143 C144 116(9) . . . . ?
C211 N2 C211 C212 166(2) 3 . . . ?
C221 N2 C211 C212 42(2) . . . . ?
C221 N2 C211 C212 -78(2) 3 . . . ?
N2 C211 C212 C213 176.4(16) . . . . ?
C211 C212 C213 C214 -147.0(19) . . . . ?
C211 N2 C221 C222 77(2) . . . . ?
C211 N2 C221 C222 -37(3) 3 . . . ?
C221 N2 C221 C222 -156(3) 3 . . . ?
N2 C221 C222 C223 159(2) . . . . ?
C221 C222 C223 C224 175(3) . . . . ?

_refine_diff_density_max         1.897
_refine_diff_density_min         -3.435
_refine_diff_density_rms         0.566

_shelxl_version_number           2014/6




loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.086 0.082 0.551 5479 5167 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Co2
_database_code_depnum_ccdc_archive 'CCDC 1883423'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H9 Co2 N5 O48 P2 W12'
_chemical_formula_weight         3881.66

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_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, -z'
'-x, y, -z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'

_cell_length_a                   19.0803(2)
_cell_length_b                   28.3426(3)
_cell_length_c                   24.8868(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13458.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      1.117
_cell_measurement_theta_max      29.459

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_F_000             6896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    10.531
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9971
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.286
_diffrn_reflns_theta_max         29.447
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.534
_diffrn_reflns_point_group_measured_fraction_full 0.539
_reflns_number_total             9971
_reflns_number_gt                8705
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.000
_reflns_Friedel_fraction_full    0.000

_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       'Rigaku CrystalClear'
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1106P)²+104.7736P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.07(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9971
_refine_ls_number_parameters     397
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1679
_refine_ls_wR_factor_gt          0.1625
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.097
_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
W1 W 0.09466(3) 0.63934(3) 0.39222(2) 0.03835(17) Uani 1 1 d . . . . .
W2 W 0.25221(3) 0.67162(4) 0.31743(3) 0.04467(19) Uani 1 1 d . . . . .
W3 W 0.25299(3) 0.67156(4) 0.18441(3) 0.0481(2) Uani 1 1 d . . . . .
W4 W -0.09677(3) 0.63978(3) 0.39123(2) 0.03765(16) Uani 1 1 d . . . . .
W5 W -0.09814(3) 0.74453(2) 0.17356(2) 0.03304(14) Uani 1 1 d . . . . .
W6 W -0.09868(3) 0.74455(3) 0.32486(2) 0.03523(15) Uani 1 1 d . . . . .
Co1 Co -0.00093(16) 0.57276(5) 0.30996(6) 0.0359(3) Uani 1 1 d . . . . .
P1 P 0.10100(11) 0.64277(8) 0.25089(16) 0.0266(4) Uani 1 1 d . . . . .
O1 O 0.0780(7) 0.5844(6) 0.3651(5) 0.063(4) Uani 1 1 d . . . . .
O2 O -0.0719(5) 0.5822(4) 0.3636(4) 0.0296(19) Uani 1 1 d . . . . .
O3 O 0.0726(4) 0.5933(2) 0.2486(5) 0.0320(13) Uani 1 1 d . . . . .
O4 O 0.1158(6) 0.6284(6) 0.4552(5) 0.053(4) Uani 1 1 d . . . . .
O5 O 0.3164(6) 0.6894(6) 0.3596(5) 0.057(4) Uani 1 1 d . . . . .
O6 O 0.3242(6) 0.6817(6) 0.1402(5) 0.060(4) Uani 1 1 d . . . . .
O7 O -0.1235(7) 0.6257(6) 0.4577(5) 0.054(4) Uani 1 1 d . . . . .
O8 O 0.0022(6) 0.6550(3) 0.4016(3) 0.0411(17) Uani 1 1 d . . . . .
O9 O 0.1916(5) 0.6386(5) 0.3624(4) 0.043(3) Uani 1 1 d . . . . .
O10 O 0.2988(4) 0.6861(4) 0.2543(5) 0.048(2) Uani 1 1 d . . . . .
O11 O -0.1931(6) 0.6410(7) 0.3609(5) 0.061(4) Uani 1 1 d . . . . .
O12 O 0.1828(3) 0.6433(3) 0.2510(5) 0.0362(15) Uani 1 1 d . . . . .
O13 O 0.0763(4) 0.6689(3) 0.3021(3) 0.0218(17) Uani 1 1 d . . . . .
O14 O -0.0777(5) 0.6667(5) 0.2999(4) 0.044(3) Uani 1 1 d . . . . .
O15 O 0.1060(5) 0.7133(4) 0.3893(4) 0.034(2) Uani 1 1 d . . . . .
O16 O -0.1966(5) 0.7233(6) 0.1822(5) 0.054(4) Uani 1 1 d . . . . .
O17 O -0.2009(5) 0.7253(5) 0.3148(4) 0.035(2) Uani 1 1 d . . . . .
O18 O -0.1055(6) 0.7061(4) 0.3885(4) 0.040(2) Uani 1 1 d . . . . .
O19 O -0.0017(6) 0.7485(3) 0.3284(3) 0.0329(15) Uani 1 1 d . . . . .
O20 O -0.0975(3) 0.7543(3) 0.2492(5) 0.0359(16) Uani 1 1 d . . . . .
O21 O -0.1177(8) 0.7996(7) 0.1543(6) 0.074(5) Uani 1 1 d . . . . .
O22 O -0.1178(5) 0.7996(4) 0.3498(4) 0.038(2) Uani 1 1 d . . . . .
C101 C 0.0000 0.4858(8) 0.2500 0.070(6) Uiso 1 2 d S . P . .
C102 C 0.0000 0.4297(13) 0.2500 0.125(13) Uiso 1 2 d S . P . .
H10A H 0.0086 0.4184 0.2858 0.187 Uiso 0.5 1 calc R U P . .
H10B H -0.0447 0.4184 0.2379 0.187 Uiso 0.5 1 calc R U P . .
H10C H 0.0361 0.4184 0.2264 0.187 Uiso 0.5 1 calc R U P . .
O101 O 0.0107(6) 0.5035(3) 0.2945(4) 0.047(2) Uiso 1 1 d . . . . .
N201 N 0.3020(6) 0.6106(4) 0.2982(5) 0.040(3) Uiso 1 1 d . . . . .
C201 C 0.3127(11) 0.5856(6) 0.2473(15) 0.077(5) Uiso 1 1 d . . . . .
C202 C 0.3481(13) 0.5381(7) 0.2598(11) 0.085(6) Uiso 1 1 d . . . . .
H20A H 0.3595 0.5366 0.2973 0.128 Uiso 1 1 calc R U . . .
H20B H 0.3166 0.5128 0.2509 0.128 Uiso 1 1 calc R U . . .
H20C H 0.3902 0.5351 0.2389 0.128 Uiso 1 1 calc R U . . .
O201 O 0.2926(6) 0.5986(4) 0.2059(5) 0.047(3) Uiso 1 1 d . . . . .
N1 N 0.2884(14) 0.7125(10) 0.5075(12) 0.108(5) Uiso 1 1 d . U . . .
C111 C 0.2497(17) 0.7067(13) 0.5663(16) 0.117(7) Uiso 1 1 d . U . . .
C112 C 0.171(2) 0.6917(13) 0.5595(15) 0.130(8) Uiso 1 1 d . U . . .
C113 C 0.1253(19) 0.7033(9) 0.6146(15) 0.133(9) Uiso 1 1 d D U . . .
C114 C 0.106(2) 0.6531(9) 0.6345(18) 0.166(14) Uiso 1 1 d D U . . .
C121 C 0.3563(16) 0.7262(11) 0.5189(12) 0.100(6) Uiso 1 1 d . U . . .
C122 C 0.4024(17) 0.7285(13) 0.4680(14) 0.113(7) Uiso 1 1 d . U . . .
C123 C 0.4808(18) 0.7463(10) 0.4861(13) 0.110(7) Uiso 1 1 d . U . . .
C124 C 0.510(2) 0.7194(11) 0.5178(13) 0.125(9) Uiso 1 1 d . U . . .
C131 C 0.2501(18) 0.7424(13) 0.4714(15) 0.117(7) Uiso 1 1 d . U . . .
C132 C 0.2393(18) 0.7897(10) 0.4925(19) 0.129(8) Uiso 1 1 d D U . . .
C133 C 0.224(2) 0.8328(10) 0.4562(13) 0.136(9) Uiso 1 1 d D U . . .
C134 C 0.206(3) 0.8768(10) 0.4905(16) 0.201(16) Uiso 1 1 d D U . . .
C141 C 0.2812(16) 0.6570(9) 0.4833(10) 0.104(6) Uiso 1 1 d D U . . .
C142 C 0.3058(18) 0.6183(7) 0.5231(9) 0.131(7) Uiso 1 1 d D U . . .
C143 C 0.2885(14) 0.5716(8) 0.4937(10) 0.139(9) Uiso 1 1 d D U . . .
C144 C 0.3349(18) 0.5657(12) 0.4430(10) 0.157(13) Uiso 1 1 d D U . . .
N2 N 0.0000 0.9063(8) 0.2500 0.086(5) Uiso 1 2 d S U P . .
C211 C 0.0631(11) 0.8724(7) 0.2557(11) 0.076(4) Uiso 1 1 d . U . . .
C212 C 0.1286(12) 0.9012(8) 0.2624(9) 0.082(5) Uiso 1 1 d . U . . .
C213 C 0.1989(14) 0.8688(8) 0.2588(12) 0.090(6) Uiso 1 1 d . U . . .
C214 C 0.2659(17) 0.8900(11) 0.2685(13) 0.111(9) Uiso 1 1 d . U . . .
C221 C -0.001(2) 0.9358(9) 0.2956(7) 0.103(5) Uiso 1 1 d D U . . .
C222 C -0.003(2) 0.9092(9) 0.3438(9) 0.135(7) Uiso 1 1 d D U . . .
C223 C -0.007(2) 0.9360(9) 0.3980(7) 0.218(16) Uiso 1 1 d D U . . .
C224 C 0.0327(19) 0.9835(9) 0.3946(16) 0.167(10) Uiso 1 1 d D U . . .


_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
W1 O4 1.648(11) . ?
W1 O1 1.727(19) . ?
W1 O8 1.835(12) . ?
W1 O9 1.994(9) . ?
W1 O15 2.109(12) . ?
W1 O13 2.419(9) . ?
W2 O5 1.690(12) . ?
W2 O16 1.809(16) 3 ?
W2 O10 1.851(11) . ?
W2 O9 1.861(10) . ?
W2 N201 2.030(13) . ?
W2 O12 2.266(10) . ?
W3 O6 1.772(12) . ?
W3 O11 1.824(15) 3 ?
W3 O17 1.820(12) 3 ?
W3 O10 1.991(13) . ?
W3 O201 2.266(11) . ?
W3 O12 2.276(11) . ?
W4 O7 1.776(11) . ?
W4 O2 1.833(10) . ?
W4 O18 1.889(12) . ?
W4 O8 1.954(12) . ?
W4 O11 1.989(13) . ?
W4 O14 2.425(10) . ?
W5 O21 1.675(19) . ?
W5 O15 1.804(12) 3 ?
W5 O19 1.909(12) 3 ?
W5 O20 1.903(11) . ?
W5 O16 1.985(11) . ?
W5 O13 2.267(8) 3 ?
W6 O22 1.719(10) . ?
W6 O19 1.856(12) . ?
W6 O20 1.903(12) . ?
W6 O18 1.927(12) . ?
W6 O17 2.041(9) . ?
W6 O14 2.326(16) . ?
Co1 O2 1.920(9) . ?
Co1 O101 2.014(9) . ?
Co1 O1 2.064(15) . ?
Co1 O3 2.082(10) 3 ?
Co1 O3 2.153(11) . ?
Co1 Co1 2.985(3) 3 ?
P1 O3 1.504(7) . ?
P1 O14 1.503(13) 3 ?
P1 O13 1.548(8) . ?
P1 O12 1.560(7) . ?
O3 Co1 2.082(10) 3 ?
O11 W3 1.824(15) 3 ?
O13 W5 2.267(8) 3 ?
O14 P1 1.503(13) 3 ?
O15 W5 1.804(12) 3 ?
O16 W2 1.809(16) 3 ?
O17 W3 1.820(12) 3 ?
O19 W5 1.909(12) 3 ?
C101 O101 1.232(13) 3 ?
C101 O101 1.232(13) . ?
C101 C102 1.59(4) . ?
C102 H10A 0.9600 . ?
C102 H10B 0.9600 . ?
C102 H10C 0.9600 . ?
N201 C201 1.47(3) . ?
C201 O201 1.16(3) . ?
C201 C202 1.54(3) . ?
C202 H20A 0.9600 . ?
C202 H20B 0.9600 . ?
C202 H20C 0.9600 . ?
N1 C121 1.38(4) . ?
N1 C131 1.44(4) . ?
N1 C111 1.65(5) . ?
N1 C141 1.69(4) . ?
C111 C112 1.56(5) . ?
C112 C113 1.66(5) . ?
C113 C114 1.5500(10) . ?
C121 C122 1.55(4) . ?
C122 C123 1.64(4) . ?
C123 C124 1.23(4) . ?
C131 C132 1.45(4) . ?
C132 C133 1.55(4) . ?
C133 C134 1.5500(10) . ?
C141 C142 1.5501(10) . ?
C142 C143 1.5500(10) . ?
C143 C144 1.5499(10) . ?
N2 C221 1.41(2) . ?
N2 C221 1.41(2) 3 ?
N2 C211 1.55(2) 3 ?
N2 C211 1.55(2) . ?
C211 C212 1.50(3) . ?
C212 C213 1.63(3) . ?
C213 C214 1.43(4) . ?
C221 C222 1.42(3) . ?
C222 C224 2.548(5) . ?
C223 C224 1.5500(11) . ?

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
O4 W1 O1 104.3(7) . . ?
O4 W1 O8 99.2(5) . . ?
O1 W1 O8 95.2(5) . . ?
O4 W1 O9 97.1(5) . . ?
O1 W1 O9 90.9(6) . . ?
O8 W1 O9 160.5(4) . . ?
O4 W1 O15 101.2(7) . . ?
O1 W1 O15 154.5(5) . . ?
O8 W1 O15 82.1(4) . . ?
O9 W1 O15 84.4(5) . . ?
O4 W1 O13 169.2(6) . . ?
O1 W1 O13 85.6(4) . . ?
O8 W1 O13 84.0(3) . . ?
O9 W1 O13 78.1(3) . . ?
O15 W1 O13 68.9(3) . . ?
O5 W2 O16 100.4(6) . 3 ?
O5 W2 O10 96.5(6) . . ?
O16 W2 O10 96.1(5) 3 . ?
O5 W2 O9 103.1(6) . . ?
O16 W2 O9 92.3(6) 3 . ?
O10 W2 O9 157.0(5) . . ?
O5 W2 N201 93.6(6) . . ?
O16 W2 N201 164.9(5) 3 . ?
O10 W2 N201 76.3(5) . . ?
O9 W2 N201 90.3(5) . . ?
O5 W2 O12 169.3(5) . . ?
O16 W2 O12 87.0(4) 3 . ?
O10 W2 O12 74.9(4) . . ?
O9 W2 O12 84.2(5) . . ?
N201 W2 O12 78.5(4) . . ?
O6 W3 O11 100.0(6) . 3 ?
O6 W3 O17 106.8(6) . 3 ?
O11 W3 O17 93.6(6) 3 3 ?
O6 W3 O10 99.9(5) . . ?
O11 W3 O10 156.0(5) 3 . ?
O17 W3 O10 93.3(4) 3 . ?
O6 W3 O201 92.2(6) . . ?
O11 W3 O201 85.4(6) 3 . ?
O17 W3 O201 160.8(4) 3 . ?
O10 W3 O201 80.6(4) . . ?
O6 W3 O12 163.8(5) . . ?
O11 W3 O12 85.1(4) 3 . ?
O17 W3 O12 88.0(4) 3 . ?
O10 W3 O12 72.2(4) . . ?
O201 W3 O12 72.7(3) . . ?
O7 W4 O2 102.9(6) . . ?
O7 W4 O18 103.4(6) . . ?
O2 W4 O18 153.6(4) . . ?
O7 W4 O8 101.8(5) . . ?
O2 W4 O8 89.8(4) . . ?
O18 W4 O8 82.5(5) . . ?
O7 W4 O11 95.3(6) . . ?
O2 W4 O11 96.4(6) . . ?
O18 W4 O11 83.6(7) . . ?
O8 W4 O11 160.1(5) . . ?
O7 W4 O14 170.5(6) . . ?
O2 W4 O14 83.7(5) . . ?
O18 W4 O14 70.5(5) . . ?
O8 W4 O14 84.8(3) . . ?
O11 W4 O14 77.1(4) . . ?
O21 W5 O15 101.0(6) . 3 ?
O21 W5 O19 99.3(6) . 3 ?
O15 W5 O19 95.2(4) 3 3 ?
O21 W5 O20 98.5(6) . . ?
O15 W5 O20 158.5(4) 3 . ?
O19 W5 O20 90.6(3) 3 . ?
O21 W5 O16 95.9(7) . . ?
O15 W5 O16 82.4(6) 3 . ?
O19 W5 O16 164.9(5) 3 . ?
O20 W5 O16 86.7(4) . . ?
O21 W5 O13 177.4(6) . 3 ?
O15 W5 O13 77.5(4) 3 3 ?
O19 W5 O13 83.0(3) 3 3 ?
O20 W5 O13 82.7(3) . 3 ?
O16 W5 O13 81.9(5) . 3 ?
O22 W6 O19 98.1(4) . . ?
O22 W6 O20 103.2(5) . . ?
O19 W6 O20 91.5(3) . . ?
O22 W6 O18 101.6(5) . . ?
O19 W6 O18 93.6(4) . . ?
O20 W6 O18 153.7(4) . . ?
O22 W6 O17 94.8(5) . . ?
O19 W6 O17 167.1(4) . . ?
O20 W6 O17 85.9(3) . . ?
O18 W6 O17 83.4(5) . . ?
O22 W6 O14 173.7(5) . . ?
O19 W6 O14 84.1(3) . . ?
O20 W6 O14 82.6(3) . . ?
O18 W6 O14 72.3(4) . . ?
O17 W6 O14 83.0(4) . . ?
O2 Co1 O101 110.3(4) . . ?
O2 Co1 O1 91.7(4) . . ?
O101 Co1 O1 101.6(6) . . ?
O2 Co1 O3 89.1(4) . 3 ?
O101 Co1 O3 102.2(4) . 3 ?
O1 Co1 O3 154.2(5) . 3 ?
O2 Co1 O3 156.1(4) . . ?
O101 Co1 O3 93.2(3) . . ?
O1 Co1 O3 87.3(5) . . ?
O3 Co1 O3 81.7(3) 3 . ?
O2 Co1 Co1 134.7(3) . 3 ?
O101 Co1 Co1 78.9(3) . 3 ?
O1 Co1 Co1 131.0(4) . 3 ?
O3 Co1 Co1 46.2(3) 3 3 ?
O3 Co1 Co1 44.2(3) . 3 ?
O3 P1 O14 106.4(7) . 3 ?
O3 P1 O13 111.5(6) . . ?
O14 P1 O13 112.8(4) 3 . ?
O3 P1 O12 111.7(4) . . ?
O14 P1 O12 107.0(6) 3 . ?
O13 P1 O12 107.4(5) . . ?
W1 O1 Co1 122.5(8) . . ?
W4 O2 Co1 124.6(5) . . ?
P1 O3 Co1 121.6(6) . 3 ?
P1 O3 Co1 117.4(6) . . ?
Co1 O3 Co1 89.6(3) 3 . ?
W1 O8 W4 149.2(5) . . ?
W2 O9 W1 142.6(6) . . ?
W2 O10 W3 119.0(4) . . ?
W3 O11 W4 145.3(10) 3 . ?
P1 O12 W2 126.1(7) . . ?
P1 O12 W3 126.3(7) . . ?
W2 O12 W3 93.6(3) . . ?
P1 O13 W5 128.0(5) . 3 ?
P1 O13 W1 123.7(5) . . ?
W5 O13 W1 93.0(3) 3 . ?
P1 O14 W6 127.0(7) 3 . ?
P1 O14 W4 127.0(8) 3 . ?
W6 O14 W4 91.3(4) . . ?
W5 O15 W1 120.6(5) 3 . ?
W2 O16 W5 143.2(9) 3 . ?
W3 O17 W6 138.1(6) 3 . ?
W4 O18 W6 125.8(6) . . ?
W6 O19 W5 172.0(4) . 3 ?
W5 O20 W6 163.2(4) . . ?
O101 C101 O101 132(2) 3 . ?
O101 C101 C102 114.0(11) 3 . ?
O101 C101 C102 114.0(11) . . ?
C101 C102 H10A 109.5 . . ?
C101 C102 H10B 109.5 . . ?
H10A C102 H10B 109.5 . . ?
C101 C102 H10C 109.5 . . ?
H10A C102 H10C 109.5 . . ?
H10B C102 H10C 109.5 . . ?
C101 O101 Co1 123.3(12) . . ?
C201 N201 W2 132.9(12) . . ?
O201 C201 N201 124.6(16) . . ?
O201 C201 C202 127(3) . . ?
N201 C201 C202 108(2) . . ?
C201 C202 H20A 109.5 . . ?
C201 C202 H20B 109.5 . . ?
H20A C202 H20B 109.5 . . ?
C201 C202 H20C 109.5 . . ?
H20A C202 H20C 109.5 . . ?
H20B C202 H20C 109.5 . . ?
C201 O201 W3 127.6(13) . . ?
C121 N1 C131 116(3) . . ?
C121 N1 C111 105(3) . . ?
C131 N1 C111 113(2) . . ?
C121 N1 C141 114(2) . . ?
C131 N1 C141 107(2) . . ?
C111 N1 C141 101(2) . . ?
C112 C111 N1 111(3) . . ?
C111 C112 C113 111(3) . . ?
C114 C113 C112 102(3) . . ?
N1 C121 C122 112(3) . . ?
C121 C122 C123 108(3) . . ?
C124 C123 C122 114(3) . . ?
C132 C131 N1 113(4) . . ?
C131 C132 C133 123(4) . . ?
C134 C133 C132 111(2) . . ?
C142 C141 N1 113.9(19) . . ?
C143 C142 C141 104(2) . . ?
C144 C143 C142 110.8(3) . . ?
C221 N2 C221 107(2) . 3 ?
C221 N2 C211 115.5(17) . 3 ?
C221 N2 C211 107.8(17) 3 3 ?
C221 N2 C211 107.8(17) . . ?
C221 N2 C211 115.5(17) 3 . ?
C211 N2 C211 103(2) 3 . ?
C212 C211 N2 108.5(16) . . ?
C211 C212 C213 111.8(18) . . ?
C214 C213 C212 119(2) . . ?
N2 C221 C222 112(2) . . ?
C221 C222 C224 88.5(19) . . ?
C223 C224 C222 34.72(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 W1 O1 Co1 142.5(7) . . . . ?
O8 W1 O1 Co1 41.6(7) . . . . ?
O9 W1 O1 Co1 -119.9(7) . . . . ?
O15 W1 O1 Co1 -41.0(17) . . . . ?
O13 W1 O1 Co1 -41.9(7) . . . . ?
O7 W4 O2 Co1 -149.6(7) . . . . ?
O18 W4 O2 Co1 25.0(14) . . . . ?
O8 W4 O2 Co1 -47.5(6) . . . . ?
O11 W4 O2 Co1 113.5(7) . . . . ?
O14 W4 O2 Co1 37.3(6) . . . . ?
O14 P1 O3 Co1 -9.6(8) 3 . . 3 ?
O13 P1 O3 Co1 113.7(7) . . . 3 ?
O12 P1 O3 Co1 -126.1(6) . . . 3 ?
O14 P1 O3 Co1 -117.7(7) 3 . . . ?
O13 P1 O3 Co1 5.6(7) . . . . ?
O12 P1 O3 Co1 125.8(6) . . . . ?
O4 W1 O8 W4 -111.3(10) . . . . ?
O1 W1 O8 W4 -5.9(9) . . . . ?
O9 W1 O8 W4 102.0(16) . . . . ?
O15 W1 O8 W4 148.6(9) . . . . ?
O13 W1 O8 W4 79.1(9) . . . . ?
O5 W2 O9 W1 115.9(12) . . . . ?
O16 W2 O9 W1 14.7(13) 3 . . . ?
O10 W2 O9 W1 -96.7(17) . . . . ?
N201 W2 O9 W1 -150.4(13) . . . . ?
O12 W2 O9 W1 -72.0(12) . . . . ?
O5 W2 O10 W3 177.8(7) . . . . ?
O16 W2 O10 W3 -81.0(6) 3 . . . ?
O9 W2 O10 W3 29.8(14) . . . . ?
N201 W2 O10 W3 85.7(6) . . . . ?
O12 W2 O10 W3 4.2(5) . . . . ?
O3 P1 O12 W2 -117.8(7) . . . . ?
O14 P1 O12 W2 126.1(8) 3 . . . ?
O13 P1 O12 W2 4.8(8) . . . . ?
O3 P1 O12 W3 113.1(7) . . . . ?
O14 P1 O12 W3 -3.1(8) 3 . . . ?
O13 P1 O12 W3 -124.4(6) . . . . ?
O3 P1 O13 W5 -177.5(5) . . . 3 ?
O14 P1 O13 W5 -57.8(7) 3 . . 3 ?
O12 P1 O13 W5 59.8(7) . . . 3 ?
O3 P1 O13 W1 55.5(6) . . . . ?
O14 P1 O13 W1 175.2(7) 3 . . . ?
O12 P1 O13 W1 -67.2(6) . . . . ?
O7 W4 O18 W6 -170.0(8) . . . . ?
O2 W4 O18 W6 15.5(16) . . . . ?
O8 W4 O18 W6 89.6(7) . . . . ?
O11 W4 O18 W6 -76.1(8) . . . . ?
O14 W4 O18 W6 2.5(6) . . . . ?
O101 C101 O101 Co1 9.9(5) 3 . . . ?
C102 C101 O101 Co1 -170.1(5) . . . . ?
W2 N201 C201 O201 1(3) . . . . ?
W2 N201 C201 C202 -173.9(13) . . . . ?
N201 C201 O201 W3 15(3) . . . . ?
C202 C201 O201 W3 -171.6(16) . . . . ?
C121 N1 C111 C112 179(3) . . . . ?
C131 N1 C111 C112 52(4) . . . . ?
C141 N1 C111 C112 -62(3) . . . . ?
N1 C111 C112 C113 -161(2) . . . . ?
C111 C112 C113 C114 -114(3) . . . . ?
C131 N1 C121 C122 -60(4) . . . . ?
C111 N1 C121 C122 174(2) . . . . ?
C141 N1 C121 C122 65(3) . . . . ?
N1 C121 C122 C123 179(3) . . . . ?
C121 C122 C123 C124 62(4) . . . . ?
C121 N1 C131 C132 -63(4) . . . . ?
C111 N1 C131 C132 58(4) . . . . ?
C141 N1 C131 C132 168(3) . . . . ?
N1 C131 C132 C133 158(3) . . . . ?
C131 C132 C133 C134 173(4) . . . . ?
C121 N1 C141 C142 63(4) . . . . ?
C131 N1 C141 C142 -168(3) . . . . ?
C111 N1 C141 C142 -50(3) . . . . ?
N1 C141 C142 C143 176(2) . . . . ?
C141 C142 C143 C144 67(3) . . . . ?
C221 N2 C211 C212 -57(3) . . . . ?
C221 N2 C211 C212 63(3) 3 . . . ?
C211 N2 C211 C212 -179(2) 3 . . . ?
N2 C211 C212 C213 -170.6(17) . . . . ?
C211 C212 C213 C214 -175(3) . . . . ?
C221 N2 C221 C222 179(4) 3 . . . ?
C211 N2 C221 C222 59(4) 3 . . . ?
C211 N2 C221 C222 -55(4) . . . . ?
N2 C221 C222 C224 164(3) . . . . ?

_refine_diff_density_max         2.102
_refine_diff_density_min         -3.262
_refine_diff_density_rms         0.549

_shelxl_version_number           2014/6




loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.131 0.154 0.156 5316 4617 ' '
2 0.072 0.000 0.000 14 10 ' '
3 0.428 0.500 0.500 13 9 ' '
4 0.572 0.500 1.000 14 10 ' '
5 0.928 0.000 0.500 13 9 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Zn2
_database_code_depnum_ccdc_archive 'CCDC 1883426'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-02-12 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H9 N5 O48 P2 W12 Zn2'
_chemical_formula_weight         3894.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_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, -z'
'-x, y, -z+1/2'
'-x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'

_cell_length_a                   19.0793(2)
_cell_length_b                   28.2796(3)
_cell_length_c                   24.9170(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13444.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9439
_cell_measurement_theta_min      1.287
_cell_measurement_theta_max      29.44

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_F_000             5692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    10.612
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9717
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_av_R_equivalents  0.059
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.287
_diffrn_reflns_theta_max         29.444
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.521
_diffrn_reflns_point_group_measured_fraction_full 0.536
_reflns_number_total             9717
_reflns_number_gt                8629
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     0.000
_reflns_Friedel_fraction_full    0.000

_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       'Rigaku CrystalClear'
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.0981P)²+44.4744P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.093(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9717
_refine_ls_number_parameters     397
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1472
_refine_ls_wR_factor_gt          0.1445
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.002
_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
W1 W 1.09454(3) 0.36087(3) 0.60825(2) 0.03623(14) Uani 1 1 d . . . . .
W2 W 0.74801(2) 0.32895(3) 0.81716(2) 0.04112(17) Uani 1 1 d . . . . .
W3 W 0.74696(2) 0.32885(3) 0.68444(2) 0.03967(16) Uani 1 1 d . . . . .
W4 W 0.90346(3) 0.36093(2) 0.60952(2) 0.03418(13) Uani 1 1 d . . . . .
W5 W 1.09824(3) 0.25545(2) 0.67334(2) 0.03249(13) Uani 1 1 d . . . . .
W6 W 0.90134(3) 0.25557(2) 0.67552(2) 0.03172(13) Uani 1 1 d . . . . .
Zn1 Zn 0.99957(11) 0.42984(4) 0.69069(4) 0.0343(2) Uani 1 1 d . . . . .
P1 P 1.10045(10) 0.35756(7) 0.74922(12) 0.0257(4) Uani 1 1 d . . . . .
O1 O 1.0723(5) 0.4175(4) 0.6362(3) 0.043(2) Uani 1 1 d . . . . .
O2 O 0.9241(4) 0.4163(4) 0.6361(3) 0.038(2) Uani 1 1 d . . . . .
O3 O 0.9282(3) 0.4074(2) 0.7495(4) 0.0326(12) Uani 1 1 d . . . . .
O4 O 1.1173(5) 0.3738(3) 0.5433(3) 0.039(2) Uani 1 1 d . . . . .
O5 O 0.6796(6) 0.3173(5) 0.8579(4) 0.060(4) Uani 1 1 d . . . . .
O6 O 0.6793(4) 0.3134(5) 0.6407(4) 0.049(3) Uani 1 1 d . . . . .
O7 O 0.8783(5) 0.3719(6) 0.5442(4) 0.072(5) Uani 1 1 d . . . . .
O8 O 1.0001(5) 0.3457(3) 0.5984(3) 0.0428(18) Uani 1 1 d . . . . .
O9 O 1.1915(4) 0.3613(4) 0.6378(3) 0.0342(19) Uani 1 1 d . . . . .
O10 O 0.7020(3) 0.3129(3) 0.7524(4) 0.0415(15) Uani 1 1 d . . . . .
O11 O 0.8066(5) 0.3612(6) 0.6401(4) 0.057(3) Uani 1 1 d . . . . .
O12 O 1.1819(3) 0.3572(2) 0.7506(4) 0.0354(13) Uani 1 1 d . . . . .
O13 O 1.0762(3) 0.3314(3) 0.6972(3) 0.0225(16) Uani 1 1 d . . . . .
O14 O 0.9235(4) 0.3331(4) 0.6999(3) 0.032(2) Uani 1 1 d . . . . .
O15 O 1.1071(5) 0.2907(4) 0.6109(3) 0.041(2) Uani 1 1 d . . . . .
O16 O 1.1986(4) 0.2756(5) 0.6828(4) 0.048(3) Uani 1 1 d . . . . .
O17 O 0.8014(4) 0.2755(4) 0.6854(3) 0.033(2) Uani 1 1 d . . . . .
O18 O 0.8951(5) 0.2913(4) 0.6113(3) 0.042(2) Uani 1 1 d . . . . .
O19 O 0.9975(6) 0.2512(2) 0.6718(2) 0.0343(14) Uani 1 1 d . . . . .
O20 O 0.9024(3) 0.2461(2) 0.7508(3) 0.0315(12) Uani 1 1 d . . . . .
O21 O 1.1158(5) 0.1988(4) 0.6516(4) 0.048(3) Uani 1 1 d . . . . .
O22 O 0.8798(4) 0.2032(4) 0.6517(4) 0.043(2) Uani 1 1 d . . . . .
N201 N 0.7014(6) 0.3907(4) 0.7042(4) 0.041(2) Uiso 1 1 d . . . . .
O201 O 0.7053(5) 0.4004(4) 0.7958(4) 0.046(2) Uiso 1 1 d . . . . .
C201 C 0.6905(7) 0.4170(4) 0.7484(9) 0.051(2) Uiso 1 1 d . . . . .
C202 C 0.6476(12) 0.4604(7) 0.7500(14) 0.103(6) Uiso 1 1 d . . . . .
H20A H 0.6384 0.4709 0.7141 0.154 Uiso 1 1 calc R U . . .
H20B H 0.6041 0.4539 0.7679 0.154 Uiso 1 1 calc R U . . .
H20C H 0.6724 0.4846 0.7692 0.154 Uiso 1 1 calc R U . . .
O101 O 1.0076(7) 0.4984(3) 0.7050(4) 0.054(2) Uiso 1 1 d . . . . .
C101 C 1.0000 0.5180(7) 0.7500 0.067(5) Uiso 1 2 d S . P . .
C102 C 1.0000 0.5706(10) 0.7500 0.106(9) Uiso 1 2 d S . P . .
H10A H 1.0061 0.5819 0.7140 0.159 Uiso 0.5 1 calc R U P . .
H10B H 0.9562 0.5819 0.7640 0.159 Uiso 0.5 1 calc R U P . .
H10C H 1.0377 0.5819 0.7720 0.159 Uiso 0.5 1 calc R U P . .
N1 N 0.7770(10) 0.2176(7) 0.5058(8) 0.083(4) Uiso 1 1 d . U . . .
C111 C 0.7469(11) 0.2447(8) 0.4735(9) 0.083(5) Uiso 1 1 d . U . . .
C112 C 0.7293(15) 0.2987(9) 0.4871(11) 0.099(6) Uiso 1 1 d D U . . .
C113 C 0.7309(15) 0.3337(11) 0.4491(13) 0.120(7) Uiso 1 1 d . U . . .
C114 C 0.718(2) 0.3872(9) 0.4694(17) 0.170(12) Uiso 1 1 d D U . . .
C121 C 0.8533(10) 0.2280(7) 0.5215(7) 0.074(4) Uiso 1 1 d . U . . .
C122 C 0.9039(12) 0.2297(9) 0.4720(9) 0.090(5) Uiso 1 1 d . U . . .
C123 C 0.9801(13) 0.2477(8) 0.4897(10) 0.103(6) Uiso 1 1 d . U . . .
C124 C 1.0146(17) 0.2167(11) 0.5257(13) 0.136(9) Uiso 1 1 d . U . . .
C131 C 0.7760(11) 0.1679(7) 0.4821(8) 0.077(4) Uiso 1 1 d . U . . .
C132 C 0.8043(11) 0.1228(7) 0.5134(9) 0.088(5) Uiso 1 1 d D U . . .
C133 C 0.7995(14) 0.0774(8) 0.4791(10) 0.116(7) Uiso 1 1 d D U . . .
C134 C 0.747(2) 0.0416(10) 0.5019(19) 0.201(15) Uiso 1 1 d D U . . .
C141 C 0.7494(11) 0.2142(8) 0.5650(11) 0.089(5) Uiso 1 1 d . U . . .
C142 C 0.6673(14) 0.1984(9) 0.5597(11) 0.106(6) Uiso 1 1 d . U . . .
C143 C 0.6314(14) 0.1971(10) 0.6170(11) 0.110(7) Uiso 1 1 d D U . . .
C144 C 0.5535(15) 0.1835(18) 0.6071(19) 0.194(14) Uiso 1 1 d D U . . .
N2 N 1.0000 0.0956(6) 0.7500 0.071(4) Uiso 1 2 d S U P . .
C211 C 1.0620(10) 0.1282(6) 0.7525(10) 0.080(4) Uiso 1 1 d . U . . .
C212 C 1.1301(11) 0.1016(7) 0.7440(12) 0.095(5) Uiso 1 1 d . U . . .
C213 C 1.1976(11) 0.1317(7) 0.7400(9) 0.085(5) Uiso 1 1 d . U . . .
C214 C 1.2677(17) 0.1044(11) 0.7439(19) 0.145(10) Uiso 1 1 d . U . . .
C221 C 0.9976(16) 0.0632(7) 0.7023(8) 0.089(4) Uiso 1 1 d . U . . .
C222 C 0.9888(16) 0.0885(9) 0.6542(12) 0.115(6) Uiso 1 1 d . U . . .
C223 C 0.9765(18) 0.0527(11) 0.6101(13) 0.139(8) Uiso 1 1 d . U . . .
C224 C 1.012(2) 0.0735(14) 0.551(2) 0.197(13) Uiso 1 1 d . U . . .


_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
W1 O4 1.715(9) . ?
W1 O1 1.796(11) . ?
W1 O8 1.869(10) . ?
W1 O9 1.992(9) . ?
W1 O15 2.000(10) . ?
W1 O13 2.394(7) . ?
W2 O5 1.687(11) . ?
W2 O16 1.821(13) 3_756 ?
W2 O9 1.851(9) 3_756 ?
W2 O10 1.892(9) . ?
W2 O201 2.242(10) . ?
W2 O12 2.297(8) 3_756 ?
W3 O6 1.746(9) . ?
W3 O11 1.831(12) . ?
W3 O17 1.831(10) . ?
W3 O10 1.950(10) . ?
W3 N201 2.014(12) . ?
W3 O12 2.259(9) 3_756 ?
W4 O7 1.726(10) . ?
W4 O2 1.746(11) . ?
W4 O8 1.913(9) . ?
W4 O18 1.977(12) . ?
W4 O11 1.999(10) . ?
W4 O14 2.417(8) . ?
W5 O21 1.725(11) . ?
W5 O15 1.856(10) . ?
W5 O20 1.909(8) 3_756 ?
W5 O19 1.926(11) . ?
W5 O16 2.011(9) . ?
W5 O13 2.268(9) . ?
W6 O22 1.649(11) . ?
W6 O19 1.841(11) . ?
W6 O20 1.895(9) . ?
W6 O18 1.896(9) . ?
W6 O17 2.003(9) . ?
W6 O14 2.315(11) . ?
Zn1 O1 1.972(9) . ?
Zn1 O101 1.978(9) . ?
Zn1 O2 2.017(10) . ?
Zn1 O3 2.100(8) . ?
Zn1 O3 2.127(9) 3_756 ?
Zn1 Zn1 2.956(2) 3_756 ?
P1 O14 1.514(9) 3_756 ?
P1 O3 1.511(6) 3_756 ?
P1 O12 1.554(6) . ?
P1 O13 1.562(8) . ?
O3 P1 1.511(6) 3_756 ?
O3 Zn1 2.127(9) 3_756 ?
O9 W2 1.851(9) 3_756 ?
O12 W3 2.259(9) 3_756 ?
O12 W2 2.297(8) 3_756 ?
O14 P1 1.514(9) 3_756 ?
O16 W2 1.821(13) 3_756 ?
O20 W5 1.909(8) 3_756 ?
N201 C201 1.34(2) . ?
O201 C201 1.30(2) . ?
C201 C202 1.48(2) . ?
C202 H20A 0.9600 . ?
C202 H20B 0.9600 . ?
C202 H20C 0.9600 . ?
O101 C101 1.259(12) . ?
C101 O101 1.258(12) 3_756 ?
C101 C102 1.49(3) . ?
C102 H10A 0.9600 . ?
C102 H10B 0.9600 . ?
C102 H10C 0.9600 . ?
N1 C111 1.25(3) . ?
N1 C131 1.52(3) . ?
N1 C121 1.54(3) . ?
N1 C141 1.57(3) . ?
C111 C112 1.60(3) . ?
C112 C113 1.37(4) . ?
C113 C114 1.62(4) . ?
C121 C122 1.57(3) . ?
C122 C123 1.60(3) . ?
C123 C124 1.42(4) . ?
C131 C132 1.59(3) . ?
C132 C133 1.544(10) . ?
C133 C134 1.538(10) . ?
C141 C142 1.63(3) . ?
C142 C143 1.58(4) . ?
C143 C144 1.556(10) . ?
N2 C221 1.50(2) 3_756 ?
N2 C221 1.50(2) . ?
N2 C211 1.50(2) . ?
N2 C211 1.50(2) 3_756 ?
C211 C212 1.52(3) . ?
C212 C213 1.55(3) . ?
C213 C214 1.55(4) . ?
C221 C222 1.41(3) . ?
C222 C223 1.51(4) . ?
C223 C224 1.71(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
O4 W1 O1 103.7(4) . . ?
O4 W1 O8 99.8(4) . . ?
O1 W1 O8 91.6(4) . . ?
O4 W1 O9 96.5(4) . . ?
O1 W1 O9 94.1(4) . . ?
O8 W1 O9 161.0(3) . . ?
O4 W1 O15 102.2(4) . . ?
O1 W1 O15 154.1(4) . . ?
O8 W1 O15 83.8(4) . . ?
O9 W1 O15 83.3(4) . . ?
O4 W1 O13 170.0(4) . . ?
O1 W1 O13 85.2(4) . . ?
O8 W1 O13 84.3(3) . . ?
O9 W1 O13 78.2(3) . . ?
O15 W1 O13 69.0(3) . . ?
O5 W2 O16 105.7(6) . 3_756 ?
O5 W2 O9 102.4(5) . 3_756 ?
O16 W2 O9 93.4(5) 3_756 3_756 ?
O5 W2 O10 96.2(4) . . ?
O16 W2 O10 93.5(4) 3_756 . ?
O9 W2 O10 157.6(4) 3_756 . ?
O5 W2 O201 92.2(5) . . ?
O16 W2 O201 161.8(4) 3_756 . ?
O9 W2 O201 85.7(4) 3_756 . ?
O10 W2 O201 81.1(4) . . ?
O5 W2 O12 164.0(4) . 3_756 ?
O16 W2 O12 87.8(4) 3_756 3_756 ?
O9 W2 O12 84.9(3) 3_756 3_756 ?
O10 W2 O12 74.1(4) . 3_756 ?
O201 W2 O12 74.0(3) . 3_756 ?
O6 W3 O11 101.9(5) . . ?
O6 W3 O17 102.8(5) . . ?
O11 W3 O17 93.9(6) . . ?
O6 W3 O10 99.2(4) . . ?
O11 W3 O10 155.9(4) . . ?
O17 W3 O10 92.7(3) . . ?
O6 W3 N201 92.9(5) . . ?
O11 W3 N201 88.9(6) . . ?
O17 W3 N201 163.0(4) . . ?
O10 W3 N201 78.4(4) . . ?
O6 W3 O12 168.8(4) . 3_756 ?
O11 W3 O12 83.2(4) . 3_756 ?
O17 W3 O12 86.6(3) . 3_756 ?
O10 W3 O12 74.0(3) . 3_756 ?
N201 W3 O12 77.1(4) . 3_756 ?
O7 W4 O2 105.0(7) . . ?
O7 W4 O8 99.9(4) . . ?
O2 W4 O8 92.3(4) . . ?
O7 W4 O18 100.2(6) . . ?
O2 W4 O18 154.7(4) . . ?
O8 W4 O18 81.7(4) . . ?
O7 W4 O11 95.8(4) . . ?
O2 W4 O11 93.5(5) . . ?
O8 W4 O11 161.2(4) . . ?
O18 W4 O11 85.5(6) . . ?
O7 W4 O14 169.2(6) . . ?
O2 W4 O14 84.4(4) . . ?
O8 W4 O14 84.8(3) . . ?
O18 W4 O14 70.6(4) . . ?
O11 W4 O14 78.1(4) . . ?
O21 W5 O15 102.6(4) . . ?
O21 W5 O20 100.5(4) . 3_756 ?
O15 W5 O20 154.9(3) . 3_756 ?
O21 W5 O19 97.4(4) . . ?
O15 W5 O19 96.2(3) . . ?
O20 W5 O19 90.3(2) 3_756 . ?
O21 W5 O16 96.6(5) . . ?
O15 W5 O16 81.9(4) . . ?
O20 W5 O16 85.9(3) 3_756 . ?
O19 W5 O16 165.9(4) . . ?
O21 W5 O13 176.8(4) . . ?
O15 W5 O13 74.2(3) . . ?
O20 W5 O13 82.6(3) 3_756 . ?
O19 W5 O13 83.1(3) . . ?
O16 W5 O13 83.0(4) . . ?
O22 W6 O19 99.8(4) . . ?
O22 W6 O20 103.4(4) . . ?
O19 W6 O20 91.7(3) . . ?
O22 W6 O18 99.1(5) . . ?
O19 W6 O18 93.2(3) . . ?
O20 W6 O18 155.8(4) . . ?
O22 W6 O17 93.5(4) . . ?
O19 W6 O17 166.7(3) . . ?
O20 W6 O17 85.9(3) . . ?
O18 W6 O17 83.9(4) . . ?
O22 W6 O14 172.7(4) . . ?
O19 W6 O14 83.9(3) . . ?
O20 W6 O14 82.7(3) . . ?
O18 W6 O14 74.3(4) . . ?
O17 W6 O14 82.8(3) . . ?
O1 Zn1 O101 104.1(5) . . ?
O1 Zn1 O2 90.2(3) . . ?
O101 Zn1 O2 111.3(4) . . ?
O1 Zn1 O3 152.0(4) . . ?
O101 Zn1 O3 102.7(4) . . ?
O2 Zn1 O3 87.2(3) . . ?
O1 Zn1 O3 88.5(4) . 3_756 ?
O101 Zn1 O3 96.7(4) . 3_756 ?
O2 Zn1 O3 151.4(3) . 3_756 ?
O3 Zn1 O3 80.9(3) . 3_756 ?
O1 Zn1 Zn1 133.2(3) . 3_756 ?
O101 Zn1 Zn1 79.6(3) . 3_756 ?
O2 Zn1 Zn1 132.7(3) . 3_756 ?
O3 Zn1 Zn1 46.0(2) . 3_756 ?
O3 Zn1 Zn1 45.3(2) 3_756 3_756 ?
O14 P1 O3 107.4(6) 3_756 3_756 ?
O14 P1 O12 106.3(5) 3_756 . ?
O3 P1 O12 111.6(4) 3_756 . ?
O14 P1 O13 112.9(3) 3_756 . ?
O3 P1 O13 110.6(5) 3_756 . ?
O12 P1 O13 108.1(4) . . ?
W1 O1 Zn1 126.2(6) . . ?
W4 O2 Zn1 125.9(5) . . ?
P1 O3 Zn1 122.1(5) 3_756 . ?
P1 O3 Zn1 119.9(5) 3_756 3_756 ?
Zn1 O3 Zn1 88.7(3) . 3_756 ?
W1 O8 W4 149.1(4) . . ?
W2 O9 W1 143.2(5) 3_756 . ?
W2 O10 W3 118.7(4) . . ?
W3 O11 W4 143.3(9) . . ?
P1 O12 W3 128.3(5) . 3_756 ?
P1 O12 W2 124.6(5) . 3_756 ?
W3 O12 W2 93.1(2) 3_756 3_756 ?
P1 O13 W5 127.7(4) . . ?
P1 O13 W1 124.0(5) . . ?
W5 O13 W1 93.4(2) . . ?
P1 O14 W6 126.6(6) 3_756 . ?
P1 O14 W4 125.7(5) 3_756 . ?
W6 O14 W4 92.0(3) . . ?
W5 O15 W1 123.3(4) . . ?
W2 O16 W5 140.2(7) 3_756 . ?
W3 O17 W6 140.4(5) . . ?
W6 O18 W4 122.9(5) . . ?
W6 O19 W5 171.6(4) . . ?
W6 O20 W5 163.8(4) . 3_756 ?
C201 N201 W3 138.3(10) . . ?
C201 O201 W2 128.2(9) . . ?
O201 C201 N201 120.7(10) . . ?
O201 C201 C202 113(2) . . ?
N201 C201 C202 125(2) . . ?
C201 C202 H20A 109.5 . . ?
C201 C202 H20B 109.5 . . ?
H20A C202 H20B 109.5 . . ?
C201 C202 H20C 109.5 . . ?
H20A C202 H20C 109.5 . . ?
H20B C202 H20C 109.5 . . ?
C101 O101 Zn1 125.7(11) . . ?
O101 C101 O101 127.7(19) 3_756 . ?
O101 C101 C102 116.1(9) 3_756 . ?
O101 C101 C102 116.1(9) . . ?
C101 C102 H10A 109.5 . . ?
C101 C102 H10B 109.5 . . ?
H10A C102 H10B 109.5 . . ?
C101 C102 H10C 109.5 . . ?
H10A C102 H10C 109.5 . . ?
H10B C102 H10C 109.5 . . ?
C111 N1 C131 108.1(19) . . ?
C111 N1 C121 118.8(19) . . ?
C131 N1 C121 106.7(16) . . ?
C111 N1 C141 119(2) . . ?
C131 N1 C141 107.7(17) . . ?
C121 N1 C141 95.1(16) . . ?
N1 C111 C112 123(2) . . ?
C113 C112 C111 123(3) . . ?
C112 C113 C114 117(3) . . ?
N1 C121 C122 112.8(16) . . ?
C121 C122 C123 110.6(18) . . ?
C124 C123 C122 114(2) . . ?
N1 C131 C132 123.1(17) . . ?
C133 C132 C131 112.0(19) . . ?
C134 C133 C132 112.5(10) . . ?
N1 C141 C142 105.2(18) . . ?
C141 C142 C143 110(2) . . ?
C144 C143 C142 106(3) . . ?
C221 N2 C221 104.7(19) 3_756 . ?
C221 N2 C211 108.6(14) 3_756 . ?
C221 N2 C211 115.6(14) . . ?
C221 N2 C211 115.6(14) 3_756 3_756 ?
C221 N2 C211 108.6(14) . 3_756 ?
C211 N2 C211 104.2(18) . 3_756 ?
N2 C211 C212 111.4(15) . . ?
C211 C212 C213 116.7(17) . . ?
C212 C213 C214 116.2(19) . . ?
C222 C221 N2 111.5(18) . . ?
C221 C222 C223 107(2) . . ?
C222 C223 C224 109(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 W1 O1 Zn1 146.1(6) . . . . ?
O8 W1 O1 Zn1 45.7(6) . . . . ?
O9 W1 O1 Zn1 -116.2(6) . . . . ?
O15 W1 O1 Zn1 -33.3(14) . . . . ?
O13 W1 O1 Zn1 -38.5(6) . . . . ?
O7 W4 O2 Zn1 -146.0(5) . . . . ?
O8 W4 O2 Zn1 -45.1(5) . . . . ?
O18 W4 O2 Zn1 30.3(12) . . . . ?
O11 W4 O2 Zn1 117.0(6) . . . . ?
O14 W4 O2 Zn1 39.4(5) . . . . ?
O4 W1 O8 W4 -111.7(8) . . . . ?
O1 W1 O8 W4 -7.5(8) . . . . ?
O9 W1 O8 W4 99.9(13) . . . . ?
O15 W1 O8 W4 147.0(8) . . . . ?
O13 W1 O8 W4 77.5(8) . . . . ?
O5 W2 O10 W3 169.3(6) . . . . ?
O16 W2 O10 W3 -84.5(5) 3_756 . . . ?
O9 W2 O10 W3 23.3(12) 3_756 . . . ?
O201 W2 O10 W3 78.0(5) . . . . ?
O12 W2 O10 W3 2.2(4) 3_756 . . . ?
O6 W3 O11 W4 -118.5(10) . . . . ?
O17 W3 O11 W4 -14.5(11) . . . . ?
O10 W3 O11 W4 90.9(18) . . . . ?
N201 W3 O11 W4 148.7(11) . . . . ?
O12 W3 O11 W4 71.6(11) 3_756 . . . ?
O14 P1 O12 W3 -2.0(7) 3_756 . . 3_756 ?
O3 P1 O12 W3 114.7(6) 3_756 . . 3_756 ?
O13 P1 O12 W3 -123.5(6) . . . 3_756 ?
O14 P1 O12 W2 126.8(6) 3_756 . . 3_756 ?
O3 P1 O12 W2 -116.4(6) 3_756 . . 3_756 ?
O13 P1 O12 W2 5.4(6) . . . 3_756 ?
O14 P1 O13 W5 -57.3(6) 3_756 . . . ?
O3 P1 O13 W5 -177.6(5) 3_756 . . . ?
O12 P1 O13 W5 60.0(6) . . . . ?
O14 P1 O13 W1 174.9(6) 3_756 . . . ?
O3 P1 O13 W1 54.6(5) 3_756 . . . ?
O12 P1 O13 W1 -67.9(5) . . . . ?
O21 W5 O15 W1 -179.1(6) . . . . ?
O20 W5 O15 W1 -22.2(12) 3_756 . . . ?
O19 W5 O15 W1 81.9(6) . . . . ?
O16 W5 O15 W1 -84.0(7) . . . . ?
O13 W5 O15 W1 0.9(5) . . . . ?
O6 W3 O17 W6 128.3(7) . . . . ?
O11 W3 O17 W6 25.1(8) . . . . ?
O10 W3 O17 W6 -131.7(7) . . . . ?
N201 W3 O17 W6 -74.0(17) . . . . ?
O12 W3 O17 W6 -57.9(7) 3_756 . . . ?
O22 W6 O18 W4 172.7(5) . . . . ?
O19 W6 O18 W4 -86.9(5) . . . . ?
O20 W6 O18 W4 14.5(12) . . . . ?
O17 W6 O18 W4 80.1(6) . . . . ?
O14 W6 O18 W4 -4.1(5) . . . . ?
O22 W6 O20 W5 -162.0(12) . . . 3_756 ?
O19 W6 O20 W5 97.5(12) . . . 3_756 ?
O18 W6 O20 W5 -4.3(17) . . . 3_756 ?
O17 W6 O20 W5 -69.4(12) . . . 3_756 ?
O14 W6 O20 W5 13.8(12) . . . 3_756 ?
W2 O201 C201 N201 -1.2(17) . . . . ?
W2 O201 C201 C202 165.8(12) . . . . ?
W3 N201 C201 O201 -8(2) . . . . ?
W3 N201 C201 C202 -173.7(14) . . . . ?
Zn1 O101 C101 O101 7.1(6) . . . 3_756 ?
Zn1 O101 C101 C102 -172.9(6) . . . . ?
C131 N1 C111 C112 173(2) . . . . ?
C121 N1 C111 C112 -66(3) . . . . ?
C141 N1 C111 C112 49(3) . . . . ?
N1 C111 C112 C113 146(3) . . . . ?
C111 C112 C113 C114 -176(3) . . . . ?
C111 N1 C121 C122 -58(3) . . . . ?
C131 N1 C121 C122 65(2) . . . . ?
C141 N1 C121 C122 174.8(18) . . . . ?
N1 C121 C122 C123 172.1(17) . . . . ?
C121 C122 C123 C124 64(3) . . . . ?
C111 N1 C131 C132 -175(2) . . . . ?
C121 N1 C131 C132 56(2) . . . . ?
C141 N1 C131 C132 -45(2) . . . . ?
N1 C131 C132 C133 -177.9(19) . . . . ?
C131 C132 C133 C134 -114(3) . . . . ?
C111 N1 C141 C142 58(3) . . . . ?
C131 N1 C141 C142 -66(2) . . . . ?
C121 N1 C141 C142 -175.2(17) . . . . ?
N1 C141 C142 C143 -176.1(19) . . . . ?
C141 C142 C143 C144 178(3) . . . . ?
C221 N2 C211 C212 68(2) 3_756 . . . ?
C221 N2 C211 C212 -50(3) . . . . ?
C211 N2 C211 C212 -169(3) 3_756 . . . ?
N2 C211 C212 C213 174.2(18) . . . . ?
C211 C212 C213 C214 167(3) . . . . ?
C221 N2 C221 C222 175(3) 3_756 . . . ?
C211 N2 C221 C222 -66(3) . . . . ?
C211 N2 C221 C222 51(3) 3_756 . . . ?
N2 C221 C222 C223 -172(2) . . . . ?
C221 C222 C223 C224 -147(3) . . . . ?

_refine_diff_density_max         1.381
_refine_diff_density_min         -3.069
_refine_diff_density_rms         0.551

_shelxl_version_number           2014/6


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.101 0.098 0.065 5396 5014 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?




