# 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_s
_database_code_depnum_ccdc_archive 'CCDC 975169'
loop_
_audit_author_name
_audit_author_address
'Jun Qian'
;Jiangsu university
China
;
_audit_update_record             
;
2019-03-28 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H56 Cl Co2 N16 O12 W'
_chemical_formula_weight         1194.07

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'
Cl Cl 0.1484 0.1585 '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'
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'
W W -0.8490 6.8722 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   12.3208(17)
_cell_length_b                   12.3208(17)
_cell_length_c                   34.355(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5215.2(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2509
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      26.018

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_F_000             2388
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    2.946
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6814
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.395
_diffrn_reflns_theta_max         26.018
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             2509
_reflns_number_gt                2224
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.0470P)²+14.1738P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2509
_refine_ls_number_parameters     146
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_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 -0.5000 -0.2500 0.1250 0.01682(13) Uani 1 4 d S T P . .
Co1 Co -0.5000 -0.5000 0.0000 0.0212(2) Uani 1 2 d S . P . .
O2 O -0.4338(3) -0.6143(3) 0.03981(9) 0.0288(7) Uani 1 1 d . . . . .
O3 O -0.6538(3) -0.5669(3) 0.00462(9) 0.0297(7) Uani 1 1 d . . . . .
N1 N -0.2512(3) -0.3115(4) 0.09611(12) 0.0368(10) Uani 1 1 d . . . . .
N2 N -0.5356(3) -0.3968(3) 0.04595(11) 0.0243(8) Uani 1 1 d . . . . .
N3 N -0.7808(3) -0.6995(3) 0.00424(13) 0.0368(10) Uani 1 1 d . . . . .
N4 N -0.3472(3) -0.6485(3) 0.09742(12) 0.0317(9) Uani 1 1 d . . . . .
C1 C -0.3370(4) -0.2906(4) 0.10655(13) 0.0236(8) Uani 1 1 d . U . . .
C2 C -0.5257(3) -0.3477(3) 0.07385(13) 0.0222(8) Uani 1 1 d . U . . .
C3 C -0.3842(4) -0.5840(4) 0.06971(13) 0.0274(9) Uani 1 1 d . U . . .
H3A H -0.3724 -0.5099 0.0727 0.033 Uiso 1 1 calc R U . . .
C4 C -0.6811(4) -0.6634(4) -0.00022(13) 0.0271(10) Uani 1 1 d . U . . .
H4A H -0.6278 -0.7128 -0.0074 0.033 Uiso 1 1 calc R U . . .
C5 C -0.2969(5) -0.6024(5) 0.13211(16) 0.0479(15) Uani 1 1 d . U . . .
H5A H -0.2746 -0.6599 0.1492 0.072 Uiso 1 1 calc R U . . .
H5B H -0.2347 -0.5603 0.1247 0.072 Uiso 1 1 calc R U . . .
H5C H -0.3482 -0.5567 0.1453 0.072 Uiso 1 1 calc R U . . .
C6 C -0.3614(5) -0.7657(5) 0.09623(17) 0.0486(15) Uani 1 1 d . U . . .
H6A H -0.3311 -0.7951 0.1197 0.073 Uiso 1 1 d R U . . .
H6B H -0.3206 -0.7913 0.0743 0.073 Uiso 1 1 d R U . . .
C7 C -0.8084(4) -0.8120(4) -0.00365(18) 0.0472(14) Uani 1 1 d . U . . .
H7A H -0.8843 -0.8233 0.0012 0.071 Uiso 1 1 calc R U . . .
H7B H -0.7925 -0.8286 -0.0304 0.071 Uiso 1 1 calc R U . . .
H7C H -0.7666 -0.8586 0.0130 0.071 Uiso 1 1 calc R U . . .
C8 C -0.8686(5) -0.6266(6) 0.0141(3) 0.084(2) Uani 1 1 d . U . . .
H8A H -0.9350 -0.6669 0.0161 0.126 Uiso 1 1 calc R U . . .
H8B H -0.8533 -0.5919 0.0385 0.126 Uiso 1 1 calc R U . . .
H8C H -0.8757 -0.5725 -0.0059 0.126 Uiso 1 1 calc R U . . .
Cl1 Cl -1.0000 -0.7500 0.1250 0.0706(11) Uani 1 4 d S T P . .
O1 O -1.0470(5) -0.6698(5) 0.1010(2) 0.108(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C2 2.153(4) 12_566 ?
W1 C2 2.153(4) 14_545 ?
W1 C2 2.153(4) 7_344 ?
W1 C2 2.153(4) . ?
W1 C1 2.164(4) . ?
W1 C1 2.164(4) 12_566 ?
W1 C1 2.164(4) 7_344 ?
W1 C1 2.164(4) 14_545 ?
Co1 O3 2.072(3) . ?
Co1 O3 2.072(3) 9_445 ?
Co1 N2 2.074(4) . ?
Co1 N2 2.074(4) 9_445 ?
Co1 O2 2.126(3) 9_445 ?
Co1 O2 2.126(3) . ?
O2 C3 1.252(5) . ?
O3 C4 1.247(5) . ?
N1 C1 1.146(6) . ?
N2 C2 1.140(6) . ?
N3 C4 1.315(6) . ?
N3 C8 1.446(7) . ?
N3 C7 1.453(6) . ?
N4 C3 1.322(6) . ?
N4 C6 1.455(7) . ?
N4 C5 1.459(7) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
Cl1 O1 1.411(6) 14_535 ?
Cl1 O1 1.411(6) 7_234 ?
Cl1 O1 1.411(6) 12_466 ?
Cl1 O1 1.411(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 W1 C2 70.6(2) 12_566 14_545 ?
C2 W1 C2 131.76(14) 12_566 7_344 ?
C2 W1 C2 131.76(14) 14_545 7_344 ?
C2 W1 C2 131.76(14) 12_566 . ?
C2 W1 C2 131.75(14) 14_545 . ?
C2 W1 C2 70.6(2) 7_344 . ?
C2 W1 C1 71.72(16) 12_566 . ?
C2 W1 C1 142.33(16) 14_545 . ?
C2 W1 C1 75.76(16) 7_344 . ?
C2 W1 C1 76.59(16) . . ?
C2 W1 C1 76.59(16) 12_566 12_566 ?
C2 W1 C1 75.76(16) 14_545 12_566 ?
C2 W1 C1 71.72(16) 7_344 12_566 ?
C2 W1 C1 142.33(16) . 12_566 ?
C1 W1 C1 94.92(7) . 12_566 ?
C2 W1 C1 142.33(16) 12_566 7_344 ?
C2 W1 C1 71.72(16) 14_545 7_344 ?
C2 W1 C1 76.59(16) 7_344 7_344 ?
C2 W1 C1 75.76(16) . 7_344 ?
C1 W1 C1 145.9(2) . 7_344 ?
C1 W1 C1 94.92(7) 12_566 7_344 ?
C2 W1 C1 75.76(16) 12_566 14_545 ?
C2 W1 C1 76.59(16) 14_545 14_545 ?
C2 W1 C1 142.33(16) 7_344 14_545 ?
C2 W1 C1 71.72(16) . 14_545 ?
C1 W1 C1 94.92(7) . 14_545 ?
C1 W1 C1 145.9(2) 12_566 14_545 ?
C1 W1 C1 94.92(7) 7_344 14_545 ?
O3 Co1 O3 180.0 . 9_445 ?
O3 Co1 N2 89.54(13) . . ?
O3 Co1 N2 90.45(13) 9_445 . ?
O3 Co1 N2 90.46(13) . 9_445 ?
O3 Co1 N2 89.55(13) 9_445 9_445 ?
N2 Co1 N2 180.0 . 9_445 ?
O3 Co1 O2 87.81(13) . 9_445 ?
O3 Co1 O2 92.19(12) 9_445 9_445 ?
N2 Co1 O2 90.15(13) . 9_445 ?
N2 Co1 O2 89.85(13) 9_445 9_445 ?
O3 Co1 O2 92.19(12) . . ?
O3 Co1 O2 87.81(13) 9_445 . ?
N2 Co1 O2 89.85(13) . . ?
N2 Co1 O2 90.15(13) 9_445 . ?
O2 Co1 O2 180.00(13) 9_445 . ?
C3 O2 Co1 121.2(3) . . ?
C4 O3 Co1 128.0(3) . . ?
C2 N2 Co1 160.5(4) . . ?
C4 N3 C8 121.0(5) . . ?
C4 N3 C7 121.3(4) . . ?
C8 N3 C7 117.5(5) . . ?
C3 N4 C6 122.4(4) . . ?
C3 N4 C5 120.0(4) . . ?
C6 N4 C5 117.5(4) . . ?
N1 C1 W1 178.7(4) . . ?
N2 C2 W1 176.9(4) . . ?
O2 C3 N4 125.4(4) . . ?
O2 C3 H3A 117.3 . . ?
N4 C3 H3A 117.3 . . ?
O3 C4 N3 124.0(4) . . ?
O3 C4 H4A 118.0 . . ?
N3 C4 H4A 118.0 . . ?
N4 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 H6A 107.6 . . ?
N4 C6 H6B 106.6 . . ?
H6A C6 H6B 109.5 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 Cl1 O1 110.0(3) 14_535 7_234 ?
O1 Cl1 O1 108.5(6) 14_535 12_466 ?
O1 Cl1 O1 110.0(3) 7_234 12_466 ?
O1 Cl1 O1 110.0(3) 14_535 . ?
O1 Cl1 O1 108.5(6) 7_234 . ?
O1 Cl1 O1 110.0(3) 12_466 . ?

_refine_diff_density_max         1.551
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.114

####################################################################### 
# 
# 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_x-final
_database_code_depnum_ccdc_archive 'CCDC 975171'
_audit_update_record             
;
2015-11-27 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Co2 N24 W'
_chemical_formula_weight         1246.69

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'
Co Co 0.3494 0.9721 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-x+1/2, y, -z+1/2'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-x+1, y+1/2, -z+1'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'x-1/2, -y, z-1/2'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'x, -y+1/2, z'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   20.048(3)
_cell_length_b                   20.048(3)
_cell_length_c                   14.995(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6026.8(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1853
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      15.2

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464
_exptl_absorpt_coefficient_mu    2.500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_T_max  0.670
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7029
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1357
_reflns_number_gt                1262
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1313P)²+31.0692P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0031(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1357
_refine_ls_number_parameters     96
_refine_ls_number_restraints     137
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0981
_refine_ls_wR_factor_ref         0.2570
_refine_ls_wR_factor_gt          0.2504
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_restrained_S_all      1.206
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.006

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.0000 0.2500 0.3750 0.05443(13) Uani 1 8 d S . .
Co1 Co 0.01749(10) 0.0000 0.5000 0.0746(8) Uani 0.50 2 d SP . .
N1 N 0.0000 0.0967(4) 0.4485(5) 0.118(2) Uani 1 2 d SU . .
N2 N 0.1011(5) 0.2500 0.5474(5) 0.140(4) Uani 1 2 d S . .
C1 C 0.0000 0.1549(4) 0.4226(5) 0.082(2) Uani 1 2 d SU . .
C2 C 0.0648(4) 0.2500 0.4848(4) 0.074(2) Uani 1 2 d SU . .
N3 N 0.08672(16) 0.0202(2) 0.5795(5) 0.38833(10) Uani 1 1 d DU . .
N4 N 0.1540(2) 0.1218(3) 0.84111(18) 0.38835(14) Uani 1 1 d DU . .
C3 C 0.07498(5) 0.00261(9) 0.6655(4) 0.38835(11) Uani 1 1 d DU . .
H3A H 0.0502 -0.0363 0.6722 0.466 Uiso 1 1 calc R . .
C4 C 0.09383(5) 0.03303(8) 0.7466(6) 0.38835(10) Uani 1 1 d DU . .
H4A H 0.0795 0.0110 0.7977 0.466 Uiso 1 1 calc R . .
C5 C 0.13082(8) 0.09135(12) 0.7621(4) 0.38835(10) Uani 1 1 d DU . .
C6 C 0.14243(18) 0.1087(3) 0.6730(4) 0.38834(10) Uani 1 1 d DU . .
H6A H 0.1671 0.1474 0.6639 0.466 Uiso 1 1 calc R . .
C7 C 0.12189(19) 0.0757(3) 0.5967(6) 0.38834(11) Uani 1 1 d DU . .
H7A H 0.1358 0.0971 0.5449 0.466 Uiso 1 1 calc R . .


_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 C1 2.036(7) 11_454 ?
W1 C1 2.036(7) 18_566 ?
W1 C1 2.036(7) 28_556 ?
W1 C1 2.036(7) . ?
W1 C2 2.098(7) 18_566 ?
W1 C2 2.098(7) . ?
W1 C2 2.098(7) 11_454 ?
W1 C2 2.098(7) 28_556 ?
Co1 Co1 0.701(4) 17_556 ?
Co1 N3 1.874(6) . ?
Co1 N3 1.874(6) 5_556 ?
Co1 N1 2.115(8) 17_556 ?
Co1 N1 2.115(8) . ?
Co1 N3 2.439(5) 17_556 ?
Co1 N3 2.439(5) 21 ?
N1 C1 1.230(11) . ?
N1 Co1 2.115(8) 17_556 ?
N2 C2 1.187(11) . ?
N3 C7 1.343(7) . ?
N3 C3 1.357(9) . ?
N3 Co1 2.439(5) 17_556 ?
N4 N4 1.252(6) 8_556 ?
N4 C5 1.411(6) . ?
C3 C4 1.411(9) . ?
C3 C7 2.024(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.404(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.400(8) . ?
C6 C7 1.385(9) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?

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
C1 W1 C1 97.06(14) 11_454 18_566 ?
C1 W1 C1 97.06(14) 11_454 28_556 ?
C1 W1 C1 139.0(4) 18_566 28_556 ?
C1 W1 C1 139.0(4) 11_454 . ?
C1 W1 C1 97.06(14) 18_566 . ?
C1 W1 C1 97.06(14) 28_556 . ?
C1 W1 C2 148.8(3) 11_454 18_566 ?
C1 W1 C2 74.03(16) 18_566 18_566 ?
C1 W1 C2 74.03(16) 28_556 18_566 ?
C1 W1 C2 72.2(3) . 18_566 ?
C1 W1 C2 74.03(16) 11_454 . ?
C1 W1 C2 148.8(3) 18_566 . ?
C1 W1 C2 72.2(3) 28_556 . ?
C1 W1 C2 74.03(16) . . ?
C2 W1 C2 128.0(2) 18_566 . ?
C1 W1 C2 74.03(16) 11_454 11_454 ?
C1 W1 C2 72.2(3) 18_566 11_454 ?
C1 W1 C2 148.8(3) 28_556 11_454 ?
C1 W1 C2 74.03(16) . 11_454 ?
C2 W1 C2 128.0(2) 18_566 11_454 ?
C2 W1 C2 76.6(4) . 11_454 ?
C1 W1 C2 72.2(3) 11_454 28_556 ?
C1 W1 C2 74.03(16) 18_566 28_556 ?
C1 W1 C2 74.03(16) 28_556 28_556 ?
C1 W1 C2 148.8(3) . 28_556 ?
C2 W1 C2 76.6(4) 18_566 28_556 ?
C2 W1 C2 128.0(2) . 28_556 ?
C2 W1 C2 128.0(2) 11_454 28_556 ?
Co1 Co1 N3 137.79(19) 17_556 . ?
Co1 Co1 N3 137.79(19) 17_556 5_556 ?
N3 Co1 N3 84.4(4) . 5_556 ?
Co1 Co1 N1 80.46(6) 17_556 17_556 ?
N3 Co1 N1 95.1(2) . 17_556 ?
N3 Co1 N1 99.1(2) 5_556 17_556 ?
Co1 Co1 N1 80.46(6) 17_556 . ?
N3 Co1 N1 99.1(2) . . ?
N3 Co1 N1 95.1(2) 5_556 . ?
N1 Co1 N1 160.92(13) 17_556 . ?
Co1 Co1 N3 31.07(16) 17_556 17_556 ?
N3 Co1 N3 168.86(7) . 17_556 ?
N3 Co1 N3 106.7(3) 5_556 17_556 ?
N1 Co1 N3 83.38(17) 17_556 17_556 ?
N1 Co1 N3 80.29(17) . 17_556 ?
Co1 Co1 N3 31.07(16) 17_556 21 ?
N3 Co1 N3 106.7(3) . 21 ?
N3 Co1 N3 168.86(7) 5_556 21 ?
N1 Co1 N3 80.29(17) 17_556 21 ?
N1 Co1 N3 83.38(17) . 21 ?
N3 Co1 N3 62.1(3) 17_556 21 ?
C1 N1 Co1 169.9(2) . . ?
C1 N1 Co1 169.9(2) . 17_556 ?
Co1 N1 Co1 19.08(13) . 17_556 ?
N1 C1 W1 177.8(7) . . ?
N2 C2 W1 179.5(7) . . ?
C7 N3 C3 97.1(6) . . ?
C7 N3 Co1 133.6(5) . . ?
C3 N3 Co1 114.8(3) . . ?
C7 N3 Co1 132.9(4) . 17_556 ?
C3 N3 Co1 105.8(2) . 17_556 ?
Co1 N3 Co1 11.14(7) . 17_556 ?
N4 N4 C5 111.5(6) 8_556 . ?
N3 C3 C4 131.3(3) . . ?
N3 C3 C7 41.2(3) . . ?
C4 C3 C7 90.1(3) . . ?
N3 C3 H3A 114.4 . . ?
C4 C3 H3A 114.4 . . ?
C7 C3 H3A 155.5 . . ?
C5 C4 C3 130.1(6) . . ?
C5 C4 H4A 114.9 . . ?
C3 C4 H4A 114.9 . . ?
C6 C5 C4 97.9(5) . . ?
C6 C5 N4 129.7(3) . . ?
C4 C5 N4 132.4(6) . . ?
C7 C6 C5 128.3(5) . . ?
C7 C6 H6A 115.8 . . ?
C5 C6 H6A 115.8 . . ?
N3 C7 C6 135.3(8) . . ?
N3 C7 C3 41.7(4) . . ?
C6 C7 C3 93.6(5) . . ?
N3 C7 H7A 112.3 . . ?
C6 C7 H7A 112.3 . . ?
C3 C7 H7A 154.1 . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.163

# SQUEEZE RESULTS (APPEND TO CIF)
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
1 -0.067 0.010 -0.009 984.9 84.5
2 0.250 0.000 -0.008 161.1 12.6
3 0.250 0.500 -0.008 161.1 12.6
4 0.750 0.000 -0.009 161.1 12.6
5 0.750 0.500 -0.008 161.1 12.6
_platon_squeeze_details          
; ?
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    Moisture-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_975170
_database_code_depnum_ccdc_archive 'CCDC 975170'
loop_
_audit_author_name
_audit_author_address
'Jun Qian'
;Jiangsu university
China
;
_audit_update_record             
;
2019-03-28 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H56 Cl Co2 Mo N16 O12'
_chemical_formula_sum            'C32 H56 Cl Co2 Mo N16 O12'
_chemical_formula_weight         1106.17

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'
Cl Cl 0.1484 0.1585 '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'
Mo Mo -1.6832 0.6857 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   12.3320(17)
_cell_length_b                   12.3320(17)
_cell_length_c                   34.230(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5205.6(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1853
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      14.99

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_F_000             2275
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    0.984
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6842
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.304
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             2520
_reflns_number_gt                2043
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_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)+(0.0510P)²+9.8594P]
 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_number_reflns         2520
_refine_ls_number_parameters     146
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_ref         0.1323
_refine_ls_wR_factor_gt          0.1228
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.000
_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
Mo1 Mo -0.5000 -0.2500 0.1250 0.0200(2) Uani 1 4 d S T P . .
Co1 Co -0.7500 -0.2500 0.2500 0.0239(2) Uani 1 2 d S . P . .
O1 O -0.8642(2) -0.1845(2) 0.21004(8) 0.0311(7) Uani 1 1 d . . . . .
O2 O -0.8165(2) -0.4039(2) 0.24564(8) 0.0319(7) Uani 1 1 d . . . . .
N1 N -0.6469(3) -0.2857(3) 0.20426(10) 0.0260(8) Uani 1 1 d . . . . .
N2 N -0.5602(4) -0.0011(3) 0.15378(11) 0.0397(10) Uani 1 1 d . . . . .
N3 N -0.8973(3) -0.0973(3) 0.15208(11) 0.0341(9) Uani 1 1 d . . . . .
N4 N -0.9488(3) -0.5306(3) 0.24584(12) 0.0376(10) Uani 1 1 d . . . . .
C1 C -0.5974(3) -0.2762(3) 0.17615(12) 0.0226(9) Uani 1 1 d . U . . .
C2 C -0.5395(3) -0.0872(4) 0.14326(11) 0.0264(9) Uani 1 1 d . U . . .
C3 C -0.8339(4) -0.1344(4) 0.18009(13) 0.0324(10) Uani 1 1 d . U . . .
H3A H -0.7598 -0.1224 0.1774 0.039 Uiso 1 1 calc R U . . .
C4 C -0.9130(4) -0.4306(3) 0.24990(12) 0.0296(10) Uani 1 1 d . U . . .
H4A H -0.9628 -0.3769 0.2563 0.036 Uiso 1 1 calc R U . . .
C5 C -1.0143(4) -0.1095(5) 0.15322(15) 0.0495(14) Uani 1 1 d . U . . .
H5A H -1.0349 -0.1446 0.1771 0.074 Uiso 1 1 calc R U . . .
H5B H -1.0375 -0.1525 0.1314 0.074 Uiso 1 1 calc R U . . .
H5C H -1.0478 -0.0393 0.1519 0.074 Uiso 1 1 calc R U . . .
C6 C -0.8517(5) -0.0448(5) 0.11750(15) 0.0530(15) Uani 1 1 d . U . . .
H6A H -0.7743 -0.0409 0.1200 0.079 Uiso 1 1 calc R U . . .
H6B H -0.8808 0.0271 0.1151 0.079 Uiso 1 1 calc R U . . .
H6C H -0.8702 -0.0861 0.0947 0.079 Uiso 1 1 calc R U . . .
C7 C -0.8759(5) -0.6180(5) 0.2362(3) 0.085(2) Uani 1 1 d . U . . .
H7A H -0.8043 -0.5895 0.2322 0.128 Uiso 1 1 calc R U . . .
H7B H -0.9003 -0.6532 0.2128 0.128 Uiso 1 1 calc R U . . .
H7C H -0.8746 -0.6694 0.2573 0.128 Uiso 1 1 calc R U . . .
C8 C -1.0621(4) -0.5594(4) 0.25302(16) 0.0496(14) Uani 1 1 d . U . . .
H8A H -1.1030 -0.4948 0.2584 0.074 Uiso 1 1 calc R U . . .
H8B H -1.0663 -0.6076 0.2750 0.074 Uiso 1 1 calc R U . . .
H8C H -1.0915 -0.5945 0.2303 0.074 Uiso 1 1 calc R U . . .
Cl1 Cl -1.0000 -0.7500 0.1250 0.0740(10) Uani 1 4 d S T P . .
O3 O -0.9532(4) -0.6686(5) 0.10049(18) 0.1108(19) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C1 2.148(4) . ?
Mo1 C1 2.148(4) 7_344 ?
Mo1 C1 2.148(4) 12_566 ?
Mo1 C1 2.148(4) 14_545 ?
Mo1 C2 2.158(5) . ?
Mo1 C2 2.158(5) 12_566 ?
Mo1 C2 2.158(5) 14_545 ?
Mo1 C2 2.158(5) 7_344 ?
Co1 N1 2.064(3) . ?
Co1 N1 2.064(3) 13_345 ?
Co1 O2 2.073(3) . ?
Co1 O2 2.073(3) 13_345 ?
Co1 O1 2.123(3) . ?
Co1 O1 2.123(3) 13_345 ?
O1 C3 1.254(5) . ?
O2 C4 1.244(5) . ?
N1 C1 1.146(5) . ?
N2 C2 1.150(5) . ?
N3 C3 1.319(6) . ?
N3 C5 1.451(6) . ?
N3 C6 1.461(6) . ?
N4 C4 1.317(5) . ?
N4 C7 1.441(7) . ?
N4 C8 1.462(6) . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9300 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
Cl1 O3 1.430(5) 7_234 ?
Cl1 O3 1.430(5) 14_535 ?
Cl1 O3 1.430(5) 12_466 ?
Cl1 O3 1.430(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
C1 Mo1 C1 70.8(2) . 7_344 ?
C1 Mo1 C1 131.65(13) . 12_566 ?
C1 Mo1 C1 131.65(13) 7_344 12_566 ?
C1 Mo1 C1 131.65(13) . 14_545 ?
C1 Mo1 C1 131.65(13) 7_344 14_545 ?
C1 Mo1 C1 70.8(2) 12_566 14_545 ?
C1 Mo1 C2 77.15(15) . . ?
C1 Mo1 C2 75.53(15) 7_344 . ?
C1 Mo1 C2 142.21(15) 12_566 . ?
C1 Mo1 C2 71.46(15) 14_545 . ?
C1 Mo1 C2 71.46(15) . 12_566 ?
C1 Mo1 C2 142.22(15) 7_344 12_566 ?
C1 Mo1 C2 77.15(15) 12_566 12_566 ?
C1 Mo1 C2 75.53(15) 14_545 12_566 ?
C2 Mo1 C2 94.81(6) . 12_566 ?
C1 Mo1 C2 142.22(15) . 14_545 ?
C1 Mo1 C2 71.46(15) 7_344 14_545 ?
C1 Mo1 C2 75.53(15) 12_566 14_545 ?
C1 Mo1 C2 77.15(15) 14_545 14_545 ?
C2 Mo1 C2 94.81(6) . 14_545 ?
C2 Mo1 C2 146.3(2) 12_566 14_545 ?
C1 Mo1 C2 75.53(15) . 7_344 ?
C1 Mo1 C2 77.15(15) 7_344 7_344 ?
C1 Mo1 C2 71.46(15) 12_566 7_344 ?
C1 Mo1 C2 142.22(15) 14_545 7_344 ?
C2 Mo1 C2 146.3(2) . 7_344 ?
C2 Mo1 C2 94.81(6) 12_566 7_344 ?
C2 Mo1 C2 94.81(6) 14_545 7_344 ?
N1 Co1 N1 180.0 . 13_345 ?
N1 Co1 O2 89.63(13) . . ?
N1 Co1 O2 90.37(13) 13_345 . ?
N1 Co1 O2 90.37(13) . 13_345 ?
N1 Co1 O2 89.63(13) 13_345 13_345 ?
O2 Co1 O2 180.00(6) . 13_345 ?
N1 Co1 O1 90.07(12) . . ?
N1 Co1 O1 89.93(12) 13_345 . ?
O2 Co1 O1 92.28(12) . . ?
O2 Co1 O1 87.72(12) 13_345 . ?
N1 Co1 O1 89.93(12) . 13_345 ?
N1 Co1 O1 90.07(12) 13_345 13_345 ?
O2 Co1 O1 87.72(12) . 13_345 ?
O2 Co1 O1 92.28(12) 13_345 13_345 ?
O1 Co1 O1 180.0 . 13_345 ?
C3 O1 Co1 121.1(3) . . ?
C4 O2 Co1 127.8(3) . . ?
C1 N1 Co1 160.6(3) . . ?
C3 N3 C5 122.3(4) . . ?
C3 N3 C6 120.9(4) . . ?
C5 N3 C6 116.7(4) . . ?
C4 N4 C7 121.0(5) . . ?
C4 N4 C8 122.0(4) . . ?
C7 N4 C8 117.0(4) . . ?
N1 C1 Mo1 176.5(4) . . ?
N2 C2 Mo1 178.6(4) . . ?
O1 C3 N3 126.0(4) . . ?
O1 C3 H3A 117.0 . . ?
N3 C3 H3A 117.0 . . ?
O2 C4 N4 123.8(4) . . ?
O2 C4 H4A 118.1 . . ?
N4 C4 H4A 118.1 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 Cl1 O3 110.1(3) 7_234 14_535 ?
O3 Cl1 O3 110.1(3) 7_234 12_466 ?
O3 Cl1 O3 108.1(5) 14_535 12_466 ?
O3 Cl1 O3 108.1(5) 7_234 . ?
O3 Cl1 O3 110.1(3) 14_535 . ?
O3 Cl1 O3 110.1(3) 12_466 . ?

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
Co1 O1 C3 N3 174.9(3) . . . . ?
C5 N3 C3 O1 0.9(7) . . . . ?
C6 N3 C3 O1 -176.9(4) . . . . ?
Co1 O2 C4 N4 178.6(3) . . . . ?
C7 N4 C4 O2 0.6(8) . . . . ?
C8 N4 C4 O2 176.9(4) . . . . ?

_refine_diff_density_max         1.435
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.091

_shelxl_version_number           2013-2

