# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_compound1
_database_code_depnum_ccdc_archive 'CCDC 2177796'
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_audit_creation_date             2021-11-15
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H64 Cl4 O22 P4 Sb4 V2'
_chemical_formula_sum            'C44 H64 Cl4 O22 P4 Sb4 V2'
_chemical_formula_weight         1799.51
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O P V Sb Cl'
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'
Cl Cl 0.1484 0.1585 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.9319(2)
_cell_length_b                   24.0942(5)
_cell_length_c                   13.5380(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.005(2)
_cell_angle_gamma                90
_cell_volume                     3199.73(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17657
_cell_measurement_temperature    109(3)
_cell_measurement_theta_max      26.8040
_cell_measurement_theta_min      2.2400
_shelx_estimated_absorpt_T_max   0.741
_shelx_estimated_absorpt_T_min   0.622
_exptl_absorpt_coefficient_mu    2.281
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29157
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.242
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  12.00   0.50   20.00    --  -14.97 -61.00  60.00   98
  2  ω    -41.00  47.00   0.50   20.00    --   16.22 -77.00  60.00  176
  3  ω     23.00  58.00   0.50   20.00    --  -14.97  30.00  90.00   70
  4  ω     12.00  37.00   0.50   20.00    --   16.22 -61.00 150.00   50
  5  ω    -40.00  17.00   0.50   20.00    --  -14.97  30.00  90.00  114
  6  ω    -53.00   4.00   0.50   20.00    --   16.22 -61.00 150.00  114
  7  ω    -54.00   0.00   0.50   20.00    --   16.22 -30.00 150.00  108
  8  ω    -75.00 -43.00   0.50   20.00    --  -14.97 -61.00  60.00   64
  9  ω    -59.00 -20.00   0.50   20.00    --  -14.97 108.00 -11.00   78
 10  ω    -36.00  10.00   0.50   20.00    --  -14.97 -94.00 -60.00   92
 11  ω    -11.00  14.00   0.50   20.00    --   16.22 -45.00 -60.00   50
 12  ω      3.00  61.00   0.50   20.00    --   16.22-108.00-109.00  116
 13  ω    -44.00 -18.00   0.50   20.00    --   16.22 -45.00 -60.00   52
 14  ω     47.00  72.00   0.50   20.00    --   16.22  45.00-150.00   50
 15  ω     -8.00  74.00   0.50   20.00    --   16.22  77.00-150.00  164
 16  ω    -61.00 -36.00   0.50   20.00    --  -14.97 125.00-120.00   50
 17  ω    -56.00 -31.00   0.50   20.00    --  -14.97 125.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0150325000
_diffrn_orient_matrix_UB_12      0.0141409000
_diffrn_orient_matrix_UB_13      -0.0463516000
_diffrn_orient_matrix_UB_21      0.0107353000
_diffrn_orient_matrix_UB_22      -0.0249097000
_diffrn_orient_matrix_UB_23      -0.0256357000
_diffrn_orient_matrix_UB_31      -0.0699037000
_diffrn_orient_matrix_UB_32      -0.0068426000
_diffrn_orient_matrix_UB_33      -0.0025493000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5014
_reflns_number_total             5855
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5855
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0377P)²+0.9113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0908
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C2(H2), C3(H3), C12(H12), C11(H11), C6(H6), C5(H5)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C14(H14A,
 H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Sb1 Sb 0.58103(3) 0.40500(2) 0.58091(2) 0.01997(10) Uani 1 1 d . . . . .
Sb2 Sb 0.64935(3) 0.48417(2) 0.36156(2) 0.01989(10) Uani 1 1 d . . . . .
V1 V 0.75120(7) 0.59416(3) 0.49608(5) 0.02425(18) Uani 1 1 d . . . . .
P1 P 0.68619(10) 0.52092(5) 0.69686(8) 0.0208(2) Uani 1 1 d . . . . .
P2 P 0.63594(11) 0.60636(5) 0.27111(8) 0.0235(3) Uani 1 1 d . . . . .
Cl1 Cl 1.03468(11) 0.20428(5) 0.67766(10) 0.0416(3) Uani 1 1 d . . . . .
Cl2 Cl 0.92254(14) 0.30904(6) 0.07453(10) 0.0531(4) Uani 1 1 d . . . . .
O4 O 0.6963(3) 0.45912(11) 0.6695(2) 0.0238(7) Uani 1 1 d . . . . .
O3 O 0.4290(2) 0.45824(11) 0.56179(19) 0.0200(6) Uani 1 1 d . . . . .
O8 O 0.8184(3) 0.52283(12) 0.4369(2) 0.0258(7) Uani 1 1 d . . . . .
O9 O 0.6477(2) 0.54314(11) 0.25122(19) 0.0215(6) Uani 1 1 d . . . . .
O2 O 0.6547(3) 0.42888(12) 0.46496(19) 0.0232(6) Uani 1 1 d . . . . .
O11 O 0.4906(3) 0.61980(12) 0.2919(2) 0.0229(6) Uani 1 1 d . . . . .
O5 O 0.5381(2) 0.53730(12) 0.7047(2) 0.0223(6) Uani 1 1 d . . . . .
O10 O 0.7414(3) 0.62459(12) 0.3577(2) 0.0255(7) Uani 1 1 d . . . . .
O1 O 0.4252(3) 0.36111(12) 0.4996(2) 0.0254(7) Uani 1 1 d . . . . .
O6 O 0.7467(3) 0.55805(12) 0.6274(2) 0.0273(7) Uani 1 1 d . . . . .
O7 O 0.8798(3) 0.63178(15) 0.5398(2) 0.0446(9) Uani 1 1 d . . . . .
C7 C 0.7419(4) 0.43010(17) 0.2702(3) 0.0199(9) Uani 1 1 d . . . . .
C1 C 0.7231(4) 0.33991(18) 0.6087(3) 0.0227(9) Uani 1 1 d . . . . .
C8 C 0.7126(4) 0.43420(19) 0.1662(3) 0.0274(10) Uani 1 1 d . . . . .
H8 H 0.655512 0.462192 0.136705 0.033 Uiso 1 1 calc R . . . .
C17 C 0.7777(4) 0.52862(18) 0.8223(3) 0.0249(10) Uani 1 1 d . . . . .
C9 C 0.7680(4) 0.39691(19) 0.1079(3) 0.0305(11) Uani 1 1 d . . . . .
H9 H 0.747203 0.399312 0.038582 0.037 Uiso 1 1 calc R . . . .
C4 C 0.9134(4) 0.25657(19) 0.6501(3) 0.0296(10) Uani 1 1 d . . . . .
C2 C 0.8563(4) 0.3475(2) 0.5943(3) 0.0338(11) Uani 1 1 d . . . . .
H2 H 0.881981 0.381356 0.569816 0.041 Uiso 1 1 calc R . . . .
C3 C 0.9526(4) 0.30597(19) 0.6154(3) 0.0325(11) Uani 1 1 d . . . . .
H3 H 1.042316 0.311713 0.605981 0.039 Uiso 1 1 calc R . . . .
C10 C 0.8541(4) 0.3560(2) 0.1506(4) 0.0330(11) Uani 1 1 d . . . . .
C20 C 0.7076(5) 0.4943(2) 0.8942(3) 0.0387(12) Uani 1 1 d . . . . .
H20A H 0.616708 0.507926 0.893813 0.058 Uiso 1 1 calc GR . . . .
H20B H 0.758101 0.497127 0.960481 0.058 Uiso 1 1 calc GR . . . .
H20C H 0.703826 0.456127 0.873391 0.058 Uiso 1 1 calc GR . . . .
C13 C 0.6605(4) 0.64208(18) 0.1583(3) 0.0264(10) Uani 1 1 d . . . . .
C15 C 0.5548(5) 0.6212(2) 0.0714(3) 0.0375(12) Uani 1 1 d . . . . .
H15A H 0.562146 0.581638 0.065921 0.056 Uiso 1 1 calc GR . . . .
H15B H 0.571053 0.638254 0.010247 0.056 Uiso 1 1 calc GR . . . .
H15C H 0.464951 0.630678 0.083601 0.056 Uiso 1 1 calc GR . . . .
C12 C 0.8287(4) 0.38824(19) 0.3122(3) 0.0323(11) Uani 1 1 d . . . . .
H12 H 0.847973 0.384969 0.381389 0.039 Uiso 1 1 calc R . . . .
C11 C 0.8868(4) 0.35148(19) 0.2532(4) 0.0343(11) Uani 1 1 d . . . . .
H11 H 0.946792 0.324217 0.281985 0.041 Uiso 1 1 calc R . . . .
C18 C 0.9241(4) 0.5084(2) 0.8273(3) 0.0392(13) Uani 1 1 d . . . . .
H18A H 0.923885 0.469841 0.809263 0.059 Uiso 1 1 calc GR . . . .
H18B H 0.972121 0.513033 0.894039 0.059 Uiso 1 1 calc GR . . . .
H18C H 0.968599 0.529536 0.781652 0.059 Uiso 1 1 calc GR . . . .
C16 C 0.8057(4) 0.6304(2) 0.1382(3) 0.0402(13) Uani 1 1 d . . . . .
H16A H 0.870035 0.640748 0.195762 0.060 Uiso 1 1 calc GR . . . .
H16B H 0.822822 0.651485 0.081374 0.060 Uiso 1 1 calc GR . . . .
H16C H 0.815073 0.591517 0.125060 0.060 Uiso 1 1 calc GR . . . .
C6 C 0.6860(4) 0.2896(2) 0.6434(4) 0.0377(12) Uani 1 1 d . . . . .
H6 H 0.596652 0.283870 0.653767 0.045 Uiso 1 1 calc R . . . .
C19 C 0.7783(5) 0.59024(18) 0.8502(3) 0.0344(11) Uani 1 1 d . . . . .
H19A H 0.819244 0.611319 0.802514 0.052 Uiso 1 1 calc GR . . . .
H19B H 0.829681 0.595367 0.915721 0.052 Uiso 1 1 calc GR . . . .
H19C H 0.686358 0.602656 0.849706 0.052 Uiso 1 1 calc GR . . . .
C22 C 0.4492(5) 0.3292(2) 0.4136(3) 0.0466(14) Uani 1 1 d . . . . .
H22A H 0.441337 0.352983 0.356079 0.070 Uiso 1 1 calc GR . . . .
H22B H 0.383187 0.299922 0.401515 0.070 Uiso 1 1 calc GR . . . .
H22C H 0.539178 0.313555 0.426128 0.070 Uiso 1 1 calc GR . . . .
C5 C 0.7812(4) 0.2472(2) 0.6631(4) 0.0410(13) Uani 1 1 d . . . . .
H5 H 0.755380 0.212761 0.684922 0.049 Uiso 1 1 calc R . . . .
C21 C 0.9408(5) 0.5236(2) 0.3919(4) 0.0563(16) Uani 1 1 d . . . . .
H21A H 0.958055 0.487054 0.368481 0.084 Uiso 1 1 calc GR . . . .
H21B H 1.016393 0.535189 0.440627 0.084 Uiso 1 1 calc GR . . . .
H21C H 0.929503 0.549027 0.336635 0.084 Uiso 1 1 calc GR . . . .
C14 C 0.6423(5) 0.70470(19) 0.1744(4) 0.0427(13) Uani 1 1 d . . . . .
H14A H 0.551161 0.711770 0.186483 0.064 Uiso 1 1 calc GR . . . .
H14B H 0.658088 0.724550 0.115761 0.064 Uiso 1 1 calc GR . . . .
H14C H 0.706216 0.716824 0.230850 0.064 Uiso 1 1 calc GR . . . .


_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
Sb1 O4 2.005(3) . ?
Sb1 O3 1.967(3) . ?
Sb1 O2 1.921(3) . ?
Sb1 O11 2.052(3) 3_666 ?
Sb1 O1 2.048(3) . ?
Sb1 C1 2.104(4) . ?
Sb2 O3 1.965(3) 3_666 ?
Sb2 O8 2.047(3) . ?
Sb2 O9 2.060(3) . ?
Sb2 O2 1.927(3) . ?
Sb2 O5 2.004(3) 3_666 ?
Sb2 C7 2.104(4) . ?
V1 O3 2.230(3) 3_666 ?
V1 O8 2.051(3) . ?
V1 O10 2.000(3) . ?
V1 O1 2.065(3) 3_666 ?
V1 O6 1.987(3) . ?
V1 O7 1.602(3) . ?
P1 O4 1.542(3) . ?
P1 O5 1.543(3) . ?
P1 O6 1.490(3) . ?
P1 C17 1.806(4) . ?
P2 O9 1.554(3) . ?
P2 O11 1.548(3) . ?
P2 O10 1.510(3) . ?
P2 C13 1.803(4) . ?
Cl1 C4 1.743(4) . ?
Cl2 C10 1.738(5) . ?
O8 C21 1.443(5) . ?
O1 C22 1.446(5) . ?
C7 C8 1.396(5) . ?
C7 C12 1.389(5) . ?
C1 C2 1.380(5) . ?
C1 C6 1.371(6) . ?
C8 C9 1.368(6) . ?
C17 C20 1.526(6) . ?
C17 C18 1.526(6) . ?
C17 C19 1.531(6) . ?
C9 C10 1.373(6) . ?
C4 C3 1.359(6) . ?
C4 C5 1.371(6) . ?
C2 C3 1.383(6) . ?
C10 C11 1.381(6) . ?
C13 C15 1.534(6) . ?
C13 C16 1.534(5) . ?
C13 C14 1.539(6) . ?
C12 C11 1.378(6) . ?
C6 C5 1.390(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
O4 Sb1 O11 85.85(11) . 3_666 ?
O4 Sb1 O1 166.00(11) . . ?
O4 Sb1 C1 94.23(13) . . ?
O3 Sb1 O4 90.53(11) . . ?
O3 Sb1 O11 86.59(11) . 3_666 ?
O3 Sb1 O1 76.46(11) . . ?
O3 Sb1 C1 171.53(13) . . ?
O2 Sb1 O4 92.25(11) . . ?
O2 Sb1 O3 94.59(11) . . ?
O2 Sb1 O11 177.78(11) . 3_666 ?
O2 Sb1 O1 93.90(11) . . ?
O2 Sb1 C1 92.23(13) . . ?
O11 Sb1 C1 86.77(13) 3_666 . ?
O1 Sb1 O11 88.20(11) . 3_666 ?
O1 Sb1 C1 98.08(13) . . ?
O3 Sb2 O8 77.12(11) 3_666 . ?
O3 Sb2 O9 86.38(10) 3_666 . ?
O3 Sb2 O5 90.11(11) 3_666 3_666 ?
O3 Sb2 C7 173.32(13) 3_666 . ?
O8 Sb2 O9 87.73(11) . . ?
O8 Sb2 C7 100.08(13) . . ?
O9 Sb2 C7 87.45(13) . . ?
O2 Sb2 O3 94.17(11) . 3_666 ?
O2 Sb2 O8 91.46(11) . . ?
O2 Sb2 O9 178.89(10) . . ?
O2 Sb2 O5 93.72(11) . 3_666 ?
O2 Sb2 C7 91.95(14) . . ?
O5 Sb2 O8 166.54(11) 3_666 . ?
O5 Sb2 O9 87.24(11) 3_666 . ?
O5 Sb2 C7 92.16(13) 3_666 . ?
O8 V1 O3 71.37(10) . 3_666 ?
O8 V1 O1 141.02(11) . 3_666 ?
O10 V1 O3 87.69(10) . 3_666 ?
O10 V1 O8 84.97(11) . . ?
O10 V1 O1 85.30(11) . 3_666 ?
O1 V1 O3 70.60(10) 3_666 3_666 ?
O6 V1 O3 86.40(11) . 3_666 ?
O6 V1 O8 92.12(12) . . ?
O6 V1 O10 173.99(12) . . ?
O6 V1 O1 93.74(11) . 3_666 ?
O7 V1 O3 178.88(13) . 3_666 ?
O7 V1 O8 109.20(15) . . ?
O7 V1 O10 93.31(14) . . ?
O7 V1 O1 108.97(15) . 3_666 ?
O7 V1 O6 92.61(14) . . ?
O4 P1 O5 111.24(16) . . ?
O4 P1 C17 106.44(18) . . ?
O5 P1 C17 104.70(17) . . ?
O6 P1 O4 112.36(16) . . ?
O6 P1 O5 111.89(16) . . ?
O6 P1 C17 109.77(18) . . ?
O9 P2 C13 107.29(18) . . ?
O11 P2 O9 109.51(16) . . ?
O11 P2 C13 107.93(18) . . ?
O10 P2 O9 110.98(16) . . ?
O10 P2 O11 110.59(16) . . ?
O10 P2 C13 110.44(18) . . ?
P1 O4 Sb1 136.01(16) . . ?
Sb1 O3 V1 103.55(12) . 3_666 ?
Sb2 O3 Sb1 138.61(14) 3_666 . ?
Sb2 O3 V1 102.89(10) 3_666 3_666 ?
Sb2 O8 V1 106.52(12) . . ?
C21 O8 Sb2 118.4(3) . . ?
C21 O8 V1 120.1(3) . . ?
P2 O9 Sb2 122.87(15) . . ?
Sb1 O2 Sb2 146.09(15) . . ?
P2 O11 Sb1 123.16(16) . 3_666 ?
P1 O5 Sb2 137.08(17) . 3_666 ?
P2 O10 V1 123.13(16) . . ?
Sb1 O1 V1 106.77(13) . 3_666 ?
C22 O1 Sb1 120.1(3) . . ?
C22 O1 V1 123.2(3) . 3_666 ?
P1 O6 V1 153.53(18) . . ?
C8 C7 Sb2 120.5(3) . . ?
C12 C7 Sb2 120.6(3) . . ?
C12 C7 C8 118.8(4) . . ?
C2 C1 Sb1 120.4(3) . . ?
C6 C1 Sb1 120.8(3) . . ?
C6 C1 C2 118.8(4) . . ?
C9 C8 C7 119.8(4) . . ?
C20 C17 P1 109.3(3) . . ?
C20 C17 C18 109.0(4) . . ?
C20 C17 C19 110.7(4) . . ?
C18 C17 P1 110.1(3) . . ?
C18 C17 C19 109.4(4) . . ?
C19 C17 P1 108.2(3) . . ?
C8 C9 C10 120.6(4) . . ?
C3 C4 Cl1 118.8(3) . . ?
C3 C4 C5 121.4(4) . . ?
C5 C4 Cl1 119.8(4) . . ?
C1 C2 C3 121.4(4) . . ?
C4 C3 C2 118.6(4) . . ?
C9 C10 Cl2 119.5(4) . . ?
C9 C10 C11 120.9(4) . . ?
C11 C10 Cl2 119.5(4) . . ?
C15 C13 P2 109.0(3) . . ?
C15 C13 C16 110.7(4) . . ?
C15 C13 C14 110.4(4) . . ?
C16 C13 P2 108.5(3) . . ?
C16 C13 C14 109.9(4) . . ?
C14 C13 P2 108.3(3) . . ?
C11 C12 C7 121.3(4) . . ?
C12 C11 C10 118.6(4) . . ?
C1 C6 C5 120.3(4) . . ?
C4 C5 C6 119.4(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.998
_oxdiff_exptl_absorpt_empirical_full_min 0.259
####################################################################### 
# 
# 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_compound5
_database_code_depnum_ccdc_archive 'CCDC 2177800'
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
# end Validation Reply Form
_audit_creation_date             2021-11-15
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C66 H102 Cu2 N2 O20 P4 Sb4, 2(C H4 O)'
_chemical_formula_sum            'C68 H110 Cu2 N2 O22 P4 Sb4'
_chemical_formula_weight         2045.53
_chemical_melting_point          ?
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'
Cu Cu 0.3201 1.2651 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8207(14)
_cell_length_b                   13.3637(15)
_cell_length_c                   13.7013(15)
_cell_angle_alpha                99.588(2)
_cell_angle_beta                 93.106(2)
_cell_angle_gamma                114.547(2)
_cell_volume                     2085.5(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8726
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.748
_shelx_estimated_absorpt_T_min   0.666
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  0.7485
_exptl_absorpt_correction_T_min  0.6662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0473 before and 0.0212 after correction.
The Ratio of minimum to maximum transmission is 0.7487.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16745
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_min         1.522
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7632
_reflns_number_total             8416
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8416
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0358P)²+1.9129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0757
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C27(H27), C25(H25), C26(H26), C15(H15), C24(H24), C5(H5), C2(H2),
 C6(H6), C12(H12), C11(H11), C3(H3), C14(H14)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C21(H21A,H21B,
 H21C), C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C34(H34A,
 H34B,H34C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
2.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Sb1 Sb 0.65743(2) 0.49800(2) 0.62893(2) 0.01546(6) Uani 1 1 d . . . . .
Sb2 Sb 0.47280(2) 0.30390(2) 0.40141(2) 0.01545(6) Uani 1 1 d . . . . .
Cu1 Cu 0.76097(3) 0.70390(3) 0.51288(3) 0.01744(9) Uani 1 1 d . . . . .
P1 P 0.76144(7) 0.75551(6) 0.73527(6) 0.01756(17) Uani 1 1 d . . . . .
P2 P 0.60080(7) 0.53271(6) 0.30702(6) 0.01632(16) Uani 1 1 d . . . . .
O2 O 0.61204(17) 0.60049(16) 0.56361(15) 0.0152(4) Uani 1 1 d . . . . .
O9 O 0.64443(18) 0.76369(17) 0.72574(15) 0.0193(4) Uani 1 1 d . . . . .
O3 O 0.80390(18) 0.56625(17) 0.56787(16) 0.0201(5) Uani 1 1 d . . . . .
O1 O 0.58692(18) 0.37201(17) 0.51888(15) 0.0186(4) Uani 1 1 d . . . . .
O8 O 0.73905(18) 0.63451(16) 0.74403(15) 0.0190(5) Uani 1 1 d . . . . .
O7 O 0.35605(18) 0.20149(17) 0.47333(15) 0.0193(5) Uani 1 1 d . . . . .
O5 O 0.57985(17) 0.41721(17) 0.33004(15) 0.0185(4) Uani 1 1 d . . . . .
O10 O 0.82915(18) 0.79194(17) 0.65073(16) 0.0202(5) Uani 1 1 d . . . . .
O4 O 0.70090(18) 0.62968(17) 0.37422(16) 0.0210(5) Uani 1 1 d . . . . .
O6 O 0.48734(18) 0.54703(17) 0.30489(16) 0.0198(5) Uani 1 1 d . . . . .
N1 N 0.9106(2) 0.7987(2) 0.46859(19) 0.0191(5) Uani 1 1 d . . . . .
O11 O 1.0202(2) 0.6689(3) 0.6919(2) 0.0513(8) Uani 1 1 d . . . . .
H11A H 0.953742 0.642486 0.663219 0.077 Uiso 1 1 calc GR . . . .
C1 C 0.7136(3) 0.4083(2) 0.7154(2) 0.0190(6) Uani 1 1 d . . . . .
C23 C 1.0126(3) 0.8153(3) 0.5151(2) 0.0246(7) Uani 1 1 d . . . . .
H23 H 1.013878 0.776351 0.565106 0.030 Uiso 1 1 calc R . . . .
C28 C 0.8414(3) 0.8459(3) 0.8537(2) 0.0230(7) Uani 1 1 d . . . . .
C19 C 0.6357(3) 0.5263(3) 0.1804(2) 0.0216(7) Uani 1 1 d . . . . .
C10 C 0.5351(3) 0.1862(3) 0.3440(2) 0.0203(6) Uani 1 1 d . . . . .
C33 C 0.3972(3) 0.1676(3) 0.5557(3) 0.0283(8) Uani 1 1 d . . . . .
H33A H 0.454188 0.141892 0.536250 0.042 Uiso 1 1 calc GR . . . .
H33B H 0.333621 0.107771 0.574709 0.042 Uiso 1 1 calc GR . . . .
H33C H 0.431311 0.230366 0.611321 0.042 Uiso 1 1 calc GR . . . .
C4 C 0.7973(3) 0.2958(3) 0.8330(3) 0.0293(8) Uani 1 1 d . . . . .
C27 C 0.9100(3) 0.8561(3) 0.3976(2) 0.0261(7) Uani 1 1 d . . . . .
H27 H 0.839144 0.842848 0.363635 0.031 Uiso 1 1 calc R . . . .
C13 C 0.6034(3) 0.0206(3) 0.2550(3) 0.0315(8) Uani 1 1 d . . . . .
C22 C 0.5349(3) 0.4293(3) 0.1097(3) 0.0312(8) Uani 1 1 d . . . . .
H22A H 0.519152 0.360370 0.131401 0.047 Uiso 1 1 calc GR . . . .
H22B H 0.555013 0.423311 0.043178 0.047 Uiso 1 1 calc GR . . . .
H22C H 0.467397 0.443480 0.110161 0.047 Uiso 1 1 calc GR . . . .
C25 C 1.1148(3) 0.9512(3) 0.4206(3) 0.0308(8) Uani 1 1 d . . . . .
H25 H 1.183437 1.003968 0.405750 0.037 Uiso 1 1 calc R . . . .
C31 C 0.7855(3) 0.7936(3) 0.9397(3) 0.0356(9) Uani 1 1 d . . . . .
H31A H 0.706413 0.782680 0.934555 0.053 Uiso 1 1 calc GR . . . .
H31B H 0.826938 0.842752 1.002210 0.053 Uiso 1 1 calc GR . . . .
H31C H 0.788234 0.722333 0.936160 0.053 Uiso 1 1 calc GR . . . .
C21 C 0.6561(4) 0.6379(3) 0.1501(3) 0.0354(9) Uani 1 1 d . . . . .
H21A H 0.586983 0.649188 0.152851 0.053 Uiso 1 1 calc GR . . . .
H21B H 0.675505 0.635626 0.083372 0.053 Uiso 1 1 calc GR . . . .
H21C H 0.718494 0.698668 0.195302 0.053 Uiso 1 1 calc GR . . . .
C32 C 0.8383(3) 0.5017(3) 0.4929(3) 0.0276(7) Uani 1 1 d . . . . .
H32A H 0.835276 0.436120 0.514935 0.041 Uiso 1 1 calc GR . . . .
H32B H 0.915872 0.546678 0.482038 0.041 Uiso 1 1 calc GR . . . .
H32C H 0.786778 0.479158 0.431676 0.041 Uiso 1 1 calc GR . . . .
C26 C 1.0094(3) 0.9339(3) 0.3725(3) 0.0302(8) Uani 1 1 d . . . . .
H26 H 1.005761 0.974146 0.324236 0.036 Uiso 1 1 calc R . . . .
C15 C 0.4578(3) 0.0722(3) 0.3207(3) 0.0325(8) Uani 1 1 d . . . . .
H15 H 0.381988 0.050128 0.333972 0.039 Uiso 1 1 calc R . . . .
C16 C 0.6333(3) -0.0711(3) 0.2014(3) 0.0376(9) Uani 1 1 d . . . . .
H16 H 0.602012 -0.134147 0.235465 0.045 Uiso 1 1 calc R . . . .
C24 C 1.1166(3) 0.8889(3) 0.4910(3) 0.0301(8) Uani 1 1 d . . . . .
H24 H 1.186560 0.896254 0.521734 0.036 Uiso 1 1 calc R . . . .
C20 C 0.7448(3) 0.5071(4) 0.1772(3) 0.0391(9) Uani 1 1 d . . . . .
H20A H 0.807279 0.567594 0.222488 0.059 Uiso 1 1 calc GR . . . .
H20B H 0.764840 0.504341 0.110570 0.059 Uiso 1 1 calc GR . . . .
H20C H 0.731022 0.437247 0.196380 0.059 Uiso 1 1 calc GR . . . .
C5 C 0.7717(3) 0.3828(3) 0.8765(3) 0.0356(9) Uani 1 1 d . . . . .
H5 H 0.782346 0.404376 0.945803 0.043 Uiso 1 1 calc R . . . .
C2 C 0.7359(3) 0.3186(3) 0.6711(3) 0.0302(8) Uani 1 1 d . . . . .
H2 H 0.722301 0.294788 0.601915 0.036 Uiso 1 1 calc R . . . .
C6 C 0.7307(3) 0.4380(3) 0.8193(3) 0.0326(8) Uani 1 1 d . . . . .
H6 H 0.714282 0.496035 0.850730 0.039 Uiso 1 1 calc R . . . .
C12 C 0.6817(3) 0.1342(3) 0.2796(3) 0.0361(9) Uani 1 1 d . . . . .
H12 H 0.757573 0.156016 0.266303 0.043 Uiso 1 1 calc R . . . .
C29 C 0.9656(3) 0.8593(3) 0.8579(3) 0.0389(9) Uani 1 1 d . . . . .
H29A H 0.966303 0.787541 0.856567 0.058 Uiso 1 1 calc GR . . . .
H29B H 1.010584 0.910719 0.918469 0.058 Uiso 1 1 calc GR . . . .
H29C H 0.998136 0.888083 0.801463 0.058 Uiso 1 1 calc GR . . . .
C11 C 0.6472(3) 0.2152(3) 0.3240(3) 0.0327(8) Uani 1 1 d . . . . .
H11 H 0.700843 0.290244 0.340425 0.039 Uiso 1 1 calc R . . . .
C3 C 0.7782(3) 0.2648(3) 0.7296(3) 0.0343(8) Uani 1 1 d . . . . .
H3 H 0.794230 0.206304 0.698685 0.041 Uiso 1 1 calc R . . . .
C34 C 1.0335(4) 0.5906(4) 0.7417(4) 0.0504(11) Uani 1 1 d . . . . .
H34A H 1.019230 0.523406 0.694127 0.076 Uiso 1 1 calc GR . . . .
H34B H 0.979401 0.572905 0.789103 0.076 Uiso 1 1 calc GR . . . .
H34C H 1.110934 0.621989 0.776152 0.076 Uiso 1 1 calc GR . . . .
C14 C 0.4925(3) -0.0082(3) 0.2782(3) 0.0390(9) Uani 1 1 d . . . . .
H14 H 0.439866 -0.083660 0.264931 0.047 Uiso 1 1 calc R . . . .
C30 C 0.8380(4) 0.9598(3) 0.8593(3) 0.0402(10) Uani 1 1 d . . . . .
H30A H 0.865992 0.988975 0.801645 0.060 Uiso 1 1 calc GR . . . .
H30B H 0.886040 1.011253 0.918653 0.060 Uiso 1 1 calc GR . . . .
H30C H 0.759810 0.950605 0.861045 0.060 Uiso 1 1 calc GR . . . .
C7 C 0.8480(4) 0.2384(3) 0.8954(3) 0.0413(10) Uani 1 1 d . . . . .
H7 H 0.841680 0.169723 0.851441 0.050 Uiso 1 1 calc R . . . .
C17 C 0.7604(4) -0.0372(3) 0.2062(3) 0.0434(10) Uani 1 1 d . . . . .
H17A H 0.793079 0.019173 0.167383 0.065 Uiso 1 1 calc GR . . . .
H17B H 0.773380 -0.101630 0.179903 0.065 Uiso 1 1 calc GR . . . .
H17C H 0.796313 -0.007384 0.274423 0.065 Uiso 1 1 calc GR . . . .
C18 C 0.5730(4) -0.1138(4) 0.0945(3) 0.0549(12) Uani 1 1 d . . . . .
H18A H 0.491237 -0.137825 0.094312 0.082 Uiso 1 1 calc GR . . . .
H18B H 0.587186 -0.176017 0.063546 0.082 Uiso 1 1 calc GR . . . .
H18C H 0.602384 -0.054542 0.058133 0.082 Uiso 1 1 calc GR . . . .
C9 C 0.7850(5) 0.2036(5) 0.9816(4) 0.0659(15) Uani 1 1 d . . . . .
H9A H 0.795488 0.269368 1.029542 0.099 Uiso 1 1 calc GR . . . .
H9B H 0.815041 0.159829 1.012351 0.099 Uiso 1 1 calc GR . . . .
H9C H 0.703982 0.159425 0.958092 0.099 Uiso 1 1 calc GR . . . .
C8 C 0.9737(5) 0.3111(7) 0.9291(7) 0.147(4) Uani 1 1 d . . . . .
H8A H 1.012795 0.327862 0.871930 0.221 Uiso 1 1 calc GR . . . .
H8B H 1.005927 0.272292 0.964974 0.221 Uiso 1 1 calc GR . . . .
H8C H 0.983376 0.379760 0.971938 0.221 Uiso 1 1 calc GR . . . .


_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
Sb1 O2 2.0074(19) . ?
Sb1 O3 2.015(2) . ?
Sb1 O1 1.915(2) . ?
Sb1 O8 2.046(2) . ?
Sb1 O6 2.016(2) 2_666 ?
Sb1 C1 2.111(3) . ?
Sb2 O2 2.013(2) 2_666 ?
Sb2 O9 2.043(2) 2_666 ?
Sb2 O1 1.926(2) . ?
Sb2 O7 1.998(2) . ?
Sb2 O5 2.011(2) . ?
Sb2 C10 2.105(3) . ?
Cu1 O2 2.076(2) . ?
Cu1 O3 2.348(2) . ?
Cu1 O7 2.326(2) 2_666 ?
Cu1 O10 1.985(2) . ?
Cu1 O4 1.940(2) . ?
Cu1 N1 2.004(3) . ?
P1 O9 1.549(2) . ?
P1 O8 1.547(2) . ?
P1 O10 1.509(2) . ?
P1 C28 1.811(3) . ?
P2 O5 1.543(2) . ?
P2 O4 1.506(2) . ?
P2 O6 1.543(2) . ?
P2 C19 1.812(3) . ?
O3 C32 1.437(4) . ?
O7 C33 1.436(4) . ?
N1 C23 1.338(4) . ?
N1 C27 1.338(4) . ?
O11 C34 1.401(5) . ?
C1 C2 1.396(5) . ?
C1 C6 1.393(5) . ?
C23 C24 1.386(5) . ?
C28 C31 1.529(4) . ?
C28 C29 1.524(5) . ?
C28 C30 1.529(5) . ?
C19 C22 1.530(4) . ?
C19 C21 1.536(5) . ?
C19 C20 1.525(5) . ?
C10 C15 1.398(4) . ?
C10 C11 1.382(5) . ?
C4 C5 1.387(5) . ?
C4 C3 1.385(5) . ?
C4 C7 1.521(5) . ?
C27 C26 1.374(5) . ?
C13 C16 1.520(5) . ?
C13 C12 1.398(5) . ?
C13 C14 1.380(5) . ?
C25 C26 1.380(5) . ?
C25 C24 1.380(5) . ?
C15 C14 1.381(5) . ?
C16 C17 1.492(5) . ?
C16 C18 1.516(6) . ?
C5 C6 1.380(5) . ?
C2 C3 1.388(5) . ?
C12 C11 1.393(5) . ?
C7 C9 1.495(6) . ?
C7 C8 1.491(7) . ?

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
O2 Sb1 O3 83.63(8) . . ?
O2 Sb1 O8 85.30(8) . . ?
O2 Sb1 O6 90.04(8) . 2_666 ?
O2 Sb1 C1 172.06(10) . . ?
O3 Sb1 O8 84.55(8) . . ?
O3 Sb1 O6 171.53(8) . 2_666 ?
O3 Sb1 C1 96.82(10) . . ?
O1 Sb1 O2 94.80(8) . . ?
O1 Sb1 O3 93.10(9) . . ?
O1 Sb1 O8 177.63(9) . . ?
O1 Sb1 O6 93.03(9) . 2_666 ?
O1 Sb1 C1 93.09(10) . . ?
O8 Sb1 C1 86.86(10) . . ?
O6 Sb1 O8 89.34(9) 2_666 . ?
O6 Sb1 C1 88.67(10) 2_666 . ?
O2 Sb2 O9 84.21(8) 2_666 2_666 ?
O2 Sb2 C10 169.33(10) 2_666 . ?
O9 Sb2 C10 85.39(10) 2_666 . ?
O1 Sb2 O2 95.64(8) . 2_666 ?
O1 Sb2 O9 177.85(8) . 2_666 ?
O1 Sb2 O7 92.71(8) . . ?
O1 Sb2 O5 88.92(9) . . ?
O1 Sb2 C10 94.84(11) . . ?
O7 Sb2 O2 82.51(8) . 2_666 ?
O7 Sb2 O9 89.39(8) . 2_666 ?
O7 Sb2 O5 173.52(8) . . ?
O7 Sb2 C10 95.03(11) . . ?
O5 Sb2 O2 91.09(8) . 2_666 ?
O5 Sb2 O9 88.94(8) . 2_666 ?
O5 Sb2 C10 91.08(10) . . ?
O2 Cu1 O3 74.34(7) . . ?
O2 Cu1 O7 73.60(7) . 2_666 ?
O7 Cu1 O3 145.29(7) 2_666 . ?
O10 Cu1 O2 91.20(8) . . ?
O10 Cu1 O3 84.12(8) . . ?
O10 Cu1 O7 83.58(8) . 2_666 ?
O10 Cu1 N1 87.46(10) . . ?
O4 Cu1 O2 92.82(8) . . ?
O4 Cu1 O3 99.63(8) . . ?
O4 Cu1 O7 94.91(8) . 2_666 ?
O4 Cu1 O10 175.12(8) . . ?
O4 Cu1 N1 88.70(10) . . ?
N1 Cu1 O2 176.02(9) . . ?
N1 Cu1 O3 101.78(9) . . ?
N1 Cu1 O7 109.94(9) . 2_666 ?
O9 P1 C28 106.02(14) . . ?
O8 P1 O9 109.15(12) . . ?
O8 P1 C28 106.37(13) . . ?
O10 P1 O9 112.38(12) . . ?
O10 P1 O8 112.13(12) . . ?
O10 P1 C28 110.45(14) . . ?
O5 P2 O6 110.10(12) . . ?
O5 P2 C19 105.18(13) . . ?
O4 P2 O5 113.52(12) . . ?
O4 P2 O6 113.14(13) . . ?
O4 P2 C19 108.00(14) . . ?
O6 P2 C19 106.30(14) . . ?
Sb1 O2 Sb2 136.38(10) . 2_666 ?
Sb1 O2 Cu1 105.12(9) . . ?
Sb2 O2 Cu1 105.06(8) 2_666 . ?
P1 O9 Sb2 123.54(12) . 2_666 ?
Sb1 O3 Cu1 95.71(8) . . ?
C32 O3 Sb1 122.78(18) . . ?
C32 O3 Cu1 114.46(18) . . ?
Sb1 O1 Sb2 145.46(12) . . ?
P1 O8 Sb1 123.23(12) . . ?
Sb2 O7 Cu1 96.99(8) . 2_666 ?
C33 O7 Sb2 118.21(18) . . ?
C33 O7 Cu1 123.6(2) . 2_666 ?
P2 O5 Sb2 138.77(13) . . ?
P1 O10 Cu1 118.23(12) . . ?
P2 O4 Cu1 143.44(13) . . ?
P2 O6 Sb1 139.86(13) . 2_666 ?
C23 N1 Cu1 121.6(2) . . ?
C23 N1 C27 118.5(3) . . ?
C27 N1 Cu1 119.6(2) . . ?
C2 C1 Sb1 121.6(2) . . ?
C6 C1 Sb1 120.6(2) . . ?
C6 C1 C2 117.8(3) . . ?
N1 C23 C24 121.9(3) . . ?
C31 C28 P1 109.8(2) . . ?
C29 C28 P1 108.2(2) . . ?
C29 C28 C31 110.3(3) . . ?
C29 C28 C30 110.6(3) . . ?
C30 C28 P1 108.2(2) . . ?
C30 C28 C31 109.7(3) . . ?
C22 C19 P2 109.4(2) . . ?
C22 C19 C21 109.7(3) . . ?
C21 C19 P2 108.9(2) . . ?
C20 C19 P2 108.6(2) . . ?
C20 C19 C22 110.0(3) . . ?
C20 C19 C21 110.3(3) . . ?
C15 C10 Sb2 118.5(2) . . ?
C11 C10 Sb2 123.8(2) . . ?
C11 C10 C15 117.6(3) . . ?
C5 C4 C7 121.7(3) . . ?
C3 C4 C5 117.5(3) . . ?
C3 C4 C7 120.8(3) . . ?
N1 C27 C26 122.9(3) . . ?
C12 C13 C16 123.3(3) . . ?
C14 C13 C16 118.9(3) . . ?
C14 C13 C12 117.8(3) . . ?
C24 C25 C26 118.9(3) . . ?
C27 C26 C25 118.6(3) . . ?
C14 C15 C10 121.0(3) . . ?
C17 C16 C13 113.7(3) . . ?
C17 C16 C18 111.6(3) . . ?
C18 C16 C13 110.5(3) . . ?
C25 C24 C23 119.1(3) . . ?
C6 C5 C4 121.5(3) . . ?
C3 C2 C1 120.4(3) . . ?
C5 C6 C1 121.1(3) . . ?
C11 C12 C13 120.6(3) . . ?
C10 C11 C12 121.4(3) . . ?
C4 C3 C2 121.8(3) . . ?
C13 C14 C15 121.6(3) . . ?
C9 C7 C4 113.9(3) . . ?
C8 C7 C4 110.1(3) . . ?
C8 C7 C9 111.3(5) . . ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT220_compound5           
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        7.7 Ratio 
RESPONSE: This alert is generated because of disorder in the structure.
;
####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 2177798'
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_audit_creation_date             2021-11-15
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C66 H102 Co2 N2 O20 P4 Sb4, 1[CH4O]'
_chemical_formula_sum            'C67 H106 Co2 N2 O21 P4 Sb4'
_chemical_formula_weight         2004.27
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.233(8)
_cell_length_b                   20.100(8)
_cell_length_c                   16.085(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.279(10)
_cell_angle_gamma                90
_cell_volume                     8156(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5290
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.38
_shelx_estimated_absorpt_T_max   0.795
_shelx_estimated_absorpt_T_min   0.676
_exptl_absorpt_coefficient_mu    1.849
_exptl_absorpt_correction_T_max  0.7949
_exptl_absorpt_correction_T_min  0.6755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS v 2.10 (Bruker, 2003) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43123
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.864
_diffrn_reflns_theta_min         1.295
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6546
_reflns_number_total             8521
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8521
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0471
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0419P)²+2.6578P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1058
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C19(H19), C23(H23), C6(H6), C20(H20), C14(H14), C12(H12), C21(H21),
 C11(H11), C5(H5), C22(H22), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C33(H33A,H33B,H33C), C25(H25A,H25B,H25C), C31(H31A,H31B,
 H31C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C26(H26A,
 H26B,H26C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C32(H32A,H32B,H32C), C9(H9A,
 H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Sb2 Sb 0.34372(2) 0.80194(2) 0.52103(2) 0.01850(10) Uani 1 1 d . . . . .
Sb1 Sb 0.27328(2) 0.71752(2) 0.34900(2) 0.01810(10) Uani 1 1 d . . . . .
Co1 Co 0.32486(3) 0.68026(3) 0.64674(4) 0.02162(17) Uani 1 1 d . . . . .
P2 P 0.34288(5) 0.82044(7) 0.71710(8) 0.0220(3) Uani 1 1 d . . . . .
P1 P 0.26185(5) 0.59960(7) 0.49246(8) 0.0208(3) Uani 1 1 d . . . . .
O10 O 0.20262(12) 0.61793(16) 0.5010(2) 0.0221(8) Uani 1 1 d . . . . .
O3 O 0.21466(11) 0.74163(16) 0.42102(19) 0.0192(7) Uani 1 1 d . . . . .
O6 O 0.28246(12) 0.83376(16) 0.72099(19) 0.0209(8) Uani 1 1 d . . . . .
O2 O 0.32569(12) 0.76471(17) 0.4143(2) 0.0227(8) Uani 1 1 d . . . . .
O4 O 0.38107(12) 0.71858(16) 0.5630(2) 0.0225(8) Uani 1 1 d . . . . .
O1 O 0.24740(12) 0.80101(16) 0.2917(2) 0.0212(8) Uani 1 1 d . . . . .
O9 O 0.28544(12) 0.63458(16) 0.41620(19) 0.0206(8) Uani 1 1 d . . . . .
O5 O 0.36380(12) 0.84527(17) 0.6328(2) 0.0229(8) Uani 1 1 d . . . . .
O7 O 0.35612(12) 0.74863(17) 0.7324(2) 0.0235(8) Uani 1 1 d . . . . .
O8 O 0.29405(12) 0.61068(17) 0.5708(2) 0.0238(8) Uani 1 1 d . . . . .
N1 N 0.36652(17) 0.6048(2) 0.7129(3) 0.0274(10) Uani 1 1 d . . . . .
C10 C 0.41148(18) 0.8470(2) 0.4739(3) 0.0197(11) Uani 1 1 d . . . . .
C1 C 0.32938(18) 0.6918(2) 0.2605(3) 0.0188(11) Uani 1 1 d . . . . .
C27 C 0.3560(2) 0.8467(3) 0.8808(3) 0.0320(13) Uani 1 1 d . . . . .
H27A H 0.317317 0.849271 0.883634 0.048 Uiso 1 1 calc GR . . . .
H27B H 0.372091 0.874040 0.925067 0.048 Uiso 1 1 calc GR . . . .
H27C H 0.367343 0.800355 0.887960 0.048 Uiso 1 1 calc GR . . . .
C33 C 0.4102(2) 0.6762(3) 0.5082(3) 0.0301(13) Uani 1 1 d . . . . .
H33A H 0.385298 0.652223 0.471372 0.045 Uiso 1 1 calc GR . . . .
H33B H 0.431021 0.644135 0.541197 0.045 Uiso 1 1 calc GR . . . .
H33C H 0.433955 0.703290 0.474867 0.045 Uiso 1 1 calc GR . . . .
C28 C 0.2628(2) 0.5119(2) 0.4669(3) 0.0247(12) Uani 1 1 d . . . . .
C15 C 0.4096(2) 0.8831(3) 0.4017(3) 0.0303(13) Uani 1 1 d . . . . .
H15 H 0.376799 0.888178 0.372263 0.036 Uiso 1 1 calc R . . . .
C24 C 0.37365(19) 0.8722(3) 0.7963(3) 0.0268(12) Uani 1 1 d . . . . .
C16 C 0.5532(2) 0.9382(3) 0.3773(4) 0.0338(14) Uani 1 1 d . . . . .
H16 H 0.542582 0.962269 0.325139 0.041 Uiso 1 1 calc R . . . .
C25 C 0.3571(2) 0.9455(3) 0.7843(3) 0.0324(14) Uani 1 1 d . . . . .
H25A H 0.369102 0.961354 0.730253 0.049 Uiso 1 1 calc GR . . . .
H25B H 0.373213 0.972676 0.828668 0.049 Uiso 1 1 calc GR . . . .
H25C H 0.318393 0.949097 0.786266 0.049 Uiso 1 1 calc GR . . . .
C19 C 0.4099(2) 0.6189(3) 0.7586(4) 0.0419(15) Uani 1 1 d . . . . .
H19 H 0.421094 0.663949 0.762562 0.050 Uiso 1 1 calc R . . . .
C23 C 0.3514(2) 0.5416(3) 0.7099(3) 0.0359(14) Uani 1 1 d . . . . .
H23 H 0.320351 0.530331 0.678536 0.043 Uiso 1 1 calc R . . . .
C31 C 0.2348(2) 0.5016(3) 0.3829(3) 0.0344(14) Uani 1 1 d . . . . .
H31A H 0.198848 0.519961 0.384711 0.052 Uiso 1 1 calc GR . . . .
H31B H 0.232845 0.453880 0.370509 0.052 Uiso 1 1 calc GR . . . .
H31C H 0.254634 0.524225 0.339591 0.052 Uiso 1 1 calc GR . . . .
C18 C 0.5742(2) 0.9896(3) 0.4387(4) 0.0405(15) Uani 1 1 d . . . . .
H18A H 0.546603 1.022743 0.448992 0.061 Uiso 1 1 calc GR . . . .
H18B H 0.605264 1.011672 0.415782 0.061 Uiso 1 1 calc GR . . . .
H18C H 0.584279 0.967640 0.491126 0.061 Uiso 1 1 calc GR . . . .
C6 C 0.3155(2) 0.6680(3) 0.1817(3) 0.0376(15) Uani 1 1 d . . . . .
H6 H 0.279190 0.660466 0.168095 0.045 Uiso 1 1 calc R . . . .
C13 C 0.5039(2) 0.9041(3) 0.4099(3) 0.0280(12) Uani 1 1 d . . . . .
C30 C 0.2336(2) 0.4729(3) 0.5338(4) 0.0389(15) Uani 1 1 d . . . . .
H30A H 0.250808 0.480884 0.588142 0.058 Uiso 1 1 calc GR . . . .
H30B H 0.234838 0.425287 0.520915 0.058 Uiso 1 1 calc GR . . . .
H30C H 0.196645 0.487627 0.535138 0.058 Uiso 1 1 calc GR . . . .
C29 C 0.3208(2) 0.4892(3) 0.4632(4) 0.0362(14) Uani 1 1 d . . . . .
H29A H 0.339674 0.516990 0.423562 0.054 Uiso 1 1 calc GR . . . .
H29B H 0.322102 0.442602 0.445266 0.054 Uiso 1 1 calc GR . . . .
H29C H 0.337643 0.493385 0.518457 0.054 Uiso 1 1 calc GR . . . .
C20 C 0.4391(2) 0.5708(4) 0.8006(4) 0.0487(17) Uani 1 1 d . . . . .
H20 H 0.469959 0.582963 0.832019 0.058 Uiso 1 1 calc R . . . .
C7 C 0.4483(2) 0.6557(4) 0.0739(4) 0.0457(17) Uani 1 1 d . . . . .
H7 H 0.482085 0.675794 0.095691 0.055 Uiso 1 1 calc R . . . .
C14 C 0.4552(2) 0.9127(3) 0.3708(3) 0.0339(14) Uani 1 1 d . . . . .
H14 H 0.452617 0.939276 0.321958 0.041 Uiso 1 1 calc R . . . .
C26 C 0.43430(19) 0.8660(3) 0.7889(4) 0.0426(16) Uani 1 1 d . . . . .
H26A H 0.444723 0.819287 0.795702 0.064 Uiso 1 1 calc GR . . . .
H26B H 0.451844 0.892858 0.832306 0.064 Uiso 1 1 calc GR . . . .
H26C H 0.444873 0.881826 0.734136 0.064 Uiso 1 1 calc GR . . . .
C4 C 0.4066(2) 0.6687(3) 0.1371(4) 0.0394(15) Uani 1 1 d . . . . .
C12 C 0.5063(2) 0.8653(3) 0.4810(3) 0.0336(14) Uani 1 1 d . . . . .
H12 H 0.539564 0.857442 0.508061 0.040 Uiso 1 1 calc R . . . .
C21 C 0.4235(3) 0.5060(4) 0.7968(4) 0.0471(17) Uani 1 1 d . . . . .
H21 H 0.442929 0.472169 0.825311 0.056 Uiso 1 1 calc R . . . .
C11 C 0.4608(2) 0.8378(3) 0.5133(3) 0.0353(14) Uani 1 1 d . . . . .
H11 H 0.463216 0.812394 0.563036 0.042 Uiso 1 1 calc R . . . .
C17 C 0.5964(2) 0.8879(3) 0.3551(4) 0.0451(16) Uani 1 1 d . . . . .
H17A H 0.626584 0.911493 0.331535 0.068 Uiso 1 1 calc GR . . . .
H17B H 0.582124 0.856114 0.314243 0.068 Uiso 1 1 calc GR . . . .
H17C H 0.608135 0.864042 0.405357 0.068 Uiso 1 1 calc GR . . . .
C5 C 0.3534(2) 0.6549(3) 0.1223(4) 0.0438(16) Uani 1 1 d . . . . .
H5 H 0.342618 0.636049 0.070449 0.053 Uiso 1 1 calc R . . . .
C22 C 0.3792(3) 0.4915(3) 0.7507(4) 0.0466(17) Uani 1 1 d . . . . .
H22 H 0.367276 0.446784 0.746524 0.056 Uiso 1 1 calc R . . . .
C2 C 0.3833(2) 0.7062(3) 0.2735(4) 0.0431(16) Uani 1 1 d . . . . .
H2 H 0.394474 0.724429 0.325489 0.052 Uiso 1 1 calc R . . . .
C3 C 0.4205(2) 0.6950(3) 0.2144(4) 0.0491(18) Uani 1 1 d . . . . .
H3 H 0.456612 0.705318 0.226539 0.059 Uiso 1 1 calc R . . . .
C8 C 0.4350(3) 0.6893(3) -0.0102(4) 0.0555(19) Uani 1 1 d . . . . .
H8A H 0.403143 0.668787 -0.034947 0.083 Uiso 1 1 calc GR . . . .
H8B H 0.464765 0.683524 -0.047611 0.083 Uiso 1 1 calc GR . . . .
H8C H 0.428660 0.736832 -0.001391 0.083 Uiso 1 1 calc GR . . . .
C32 C 0.2831(2) 0.8510(3) 0.2677(4) 0.057(2) Uani 1 1 d . . . . .
H32A H 0.286098 0.884610 0.311751 0.086 Uiso 1 1 calc GR . . . .
H32B H 0.269928 0.872046 0.216268 0.086 Uiso 1 1 calc GR . . . .
H32C H 0.317921 0.831272 0.258411 0.086 Uiso 1 1 calc GR . . . .
C9 C 0.4583(3) 0.5814(4) 0.0612(5) 0.067(2) Uani 1 1 d . . . . .
H9A H 0.468703 0.560980 0.114461 0.101 Uiso 1 1 calc GR . . . .
H9B H 0.486788 0.575357 0.021437 0.101 Uiso 1 1 calc GR . . . .
H9C H 0.425877 0.560124 0.039569 0.101 Uiso 1 1 calc GR . . . .


_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
Sb2 O10 2.017(3) 7_566 ?
Sb2 O3 1.967(3) 7_566 ?
Sb2 O2 1.918(3) . ?
Sb2 O4 2.031(3) . ?
Sb2 O5 2.050(3) . ?
Sb2 C10 2.092(5) . ?
Sb1 O3 1.960(3) . ?
Sb1 O6 2.059(3) 7_566 ?
Sb1 O2 1.921(3) . ?
Sb1 O1 2.016(3) . ?
Sb1 O9 2.007(3) . ?
Sb1 C1 2.095(5) . ?
Co1 O3 2.145(3) 7_566 ?
Co1 O4 2.122(3) . ?
Co1 O1 2.127(3) 7_566 ?
Co1 O7 2.088(3) . ?
Co1 O8 2.003(3) . ?
Co1 N1 2.118(4) . ?
P2 O6 1.550(3) . ?
P2 O5 1.549(3) . ?
P2 O7 1.501(4) . ?
P2 C24 1.807(5) . ?
P1 O10 1.548(3) . ?
P1 O9 1.545(3) . ?
P1 O8 1.500(3) . ?
P1 C28 1.811(5) . ?
O4 C33 1.439(6) . ?
O1 C32 1.409(7) . ?
N1 C19 1.335(7) . ?
N1 C23 1.327(7) . ?
C10 C15 1.369(7) . ?
C10 C11 1.397(7) . ?
C1 C6 1.392(7) . ?
C1 C2 1.402(7) . ?
C27 C24 1.528(7) . ?
C28 C31 1.525(7) . ?
C28 C30 1.531(7) . ?
C28 C29 1.536(7) . ?
C15 C14 1.397(7) . ?
C24 C25 1.543(7) . ?
C24 C26 1.543(7) . ?
C16 C18 1.516(7) . ?
C16 C13 1.524(7) . ?
C16 C17 1.535(7) . ?
C19 C20 1.383(8) . ?
C23 C22 1.385(8) . ?
C6 C5 1.393(7) . ?
C13 C14 1.381(7) . ?
C13 C12 1.384(7) . ?
C20 C21 1.362(9) . ?
C7 C4 1.502(8) . ?
C7 C8 1.541(9) . ?
C7 C9 1.531(9) . ?
C4 C5 1.385(7) . ?
C4 C3 1.389(8) . ?
C12 C11 1.385(7) . ?
C21 C22 1.359(8) . ?
C2 C3 1.370(7) . ?

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
O10 Sb2 O4 168.60(13) 7_566 . ?
O10 Sb2 O5 86.90(13) 7_566 . ?
O10 Sb2 C10 93.78(17) 7_566 . ?
O3 Sb2 O10 90.09(13) 7_566 7_566 ?
O3 Sb2 O4 79.74(13) 7_566 . ?
O3 Sb2 O5 86.95(13) 7_566 . ?
O3 Sb2 C10 172.56(16) 7_566 . ?
O2 Sb2 O10 91.66(14) . 7_566 ?
O2 Sb2 O3 94.88(13) . 7_566 ?
O2 Sb2 O4 94.30(14) . . ?
O2 Sb2 O5 177.67(14) . . ?
O2 Sb2 C10 91.36(16) . . ?
O4 Sb2 O5 87.43(13) . . ?
O4 Sb2 C10 95.78(17) . . ?
O5 Sb2 C10 86.91(15) . . ?
O3 Sb1 O6 86.08(13) . 7_566 ?
O3 Sb1 O1 79.81(13) . . ?
O3 Sb1 O9 89.74(13) . . ?
O3 Sb1 C1 173.26(16) . . ?
O6 Sb1 C1 88.20(15) 7_566 . ?
O2 Sb1 O3 94.24(13) . . ?
O2 Sb1 O6 179.51(14) . 7_566 ?
O2 Sb1 O1 92.91(14) . . ?
O2 Sb1 O9 91.18(14) . . ?
O2 Sb1 C1 91.50(16) . . ?
O1 Sb1 O6 87.51(13) . 7_566 ?
O1 Sb1 C1 96.40(16) . . ?
O9 Sb1 O6 88.45(13) . 7_566 ?
O9 Sb1 O1 169.02(12) . . ?
O9 Sb1 C1 93.67(16) . . ?
O4 Co1 O3 73.84(12) . 7_566 ?
O4 Co1 O1 145.36(13) . 7_566 ?
O1 Co1 O3 73.33(12) 7_566 7_566 ?
O7 Co1 O3 91.04(13) . 7_566 ?
O7 Co1 O4 86.10(13) . . ?
O7 Co1 O1 83.78(13) . 7_566 ?
O7 Co1 N1 87.93(16) . . ?
O8 Co1 O3 91.79(13) . 7_566 ?
O8 Co1 O4 97.01(13) . . ?
O8 Co1 O1 94.72(13) . 7_566 ?
O8 Co1 O7 176.28(13) . . ?
O8 Co1 N1 89.32(16) . . ?
N1 Co1 O3 177.95(14) . 7_566 ?
N1 Co1 O4 104.32(15) . . ?
N1 Co1 O1 108.30(14) . 7_566 ?
O6 P2 C24 106.2(2) . . ?
O5 P2 O6 109.53(19) . . ?
O5 P2 C24 106.4(2) . . ?
O7 P2 O6 112.03(19) . . ?
O7 P2 O5 111.99(19) . . ?
O7 P2 C24 110.3(2) . . ?
O10 P1 C28 105.6(2) . . ?
O9 P1 O10 110.62(19) . . ?
O9 P1 C28 104.8(2) . . ?
O8 P1 O10 113.30(19) . . ?
O8 P1 O9 112.84(19) . . ?
O8 P1 C28 109.0(2) . . ?
P1 O10 Sb2 137.0(2) . 7_566 ?
Sb2 O3 Co1 102.84(13) 7_566 7_566 ?
Sb1 O3 Sb2 138.87(18) . 7_566 ?
Sb1 O3 Co1 103.25(14) . 7_566 ?
P2 O6 Sb1 123.50(19) . 7_566 ?
Sb2 O2 Sb1 145.98(17) . . ?
Sb2 O4 Co1 101.47(14) . . ?
C33 O4 Sb2 121.6(3) . . ?
C33 O4 Co1 122.1(3) . . ?
Sb1 O1 Co1 101.95(14) . 7_566 ?
C32 O1 Sb1 121.1(3) . . ?
C32 O1 Co1 124.1(4) . 7_566 ?
P1 O9 Sb1 138.5(2) . . ?
P2 O5 Sb2 123.25(19) . . ?
P2 O7 Co1 116.45(19) . . ?
P1 O8 Co1 144.3(2) . . ?
C19 N1 Co1 121.1(4) . . ?
C23 N1 Co1 121.9(4) . . ?
C23 N1 C19 117.0(5) . . ?
C15 C10 Sb2 121.6(4) . . ?
C15 C10 C11 117.9(5) . . ?
C11 C10 Sb2 120.4(4) . . ?
C6 C1 Sb1 122.9(4) . . ?
C6 C1 C2 115.5(5) . . ?
C2 C1 Sb1 121.0(4) . . ?
C31 C28 P1 109.0(4) . . ?
C31 C28 C30 109.5(4) . . ?
C31 C28 C29 110.4(4) . . ?
C30 C28 P1 109.3(4) . . ?
C30 C28 C29 110.4(5) . . ?
C29 C28 P1 108.4(3) . . ?
C10 C15 C14 121.0(5) . . ?
C27 C24 P2 107.7(4) . . ?
C27 C24 C25 110.4(4) . . ?
C27 C24 C26 110.5(5) . . ?
C25 C24 P2 110.5(4) . . ?
C26 C24 P2 108.1(4) . . ?
C26 C24 C25 109.5(5) . . ?
C18 C16 C13 111.0(4) . . ?
C18 C16 C17 111.2(5) . . ?
C13 C16 C17 111.8(5) . . ?
N1 C19 C20 122.9(6) . . ?
N1 C23 C22 122.5(6) . . ?
C1 C6 C5 121.8(5) . . ?
C14 C13 C16 120.7(5) . . ?
C14 C13 C12 118.0(5) . . ?
C12 C13 C16 121.2(5) . . ?
C21 C20 C19 119.7(6) . . ?
C4 C7 C8 112.1(5) . . ?
C4 C7 C9 112.4(5) . . ?
C9 C7 C8 110.1(6) . . ?
C13 C14 C15 121.1(5) . . ?
C5 C4 C7 122.6(5) . . ?
C5 C4 C3 117.1(5) . . ?
C3 C4 C7 120.3(5) . . ?
C13 C12 C11 120.9(5) . . ?
C22 C21 C20 117.6(6) . . ?
C12 C11 C10 121.0(5) . . ?
C4 C5 C6 121.4(5) . . ?
C21 C22 C23 120.3(6) . . ?
C3 C2 C1 122.7(5) . . ?
C2 C3 C4 121.3(6) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.224 0.750 36.1 2.5 ?
2 0.000 0.285 0.250 23.1 0.9 ?
3 0.000 0.715 0.750 23.1 0.9 ?
4 0.000 0.776 0.250 36.1 2.5 ?
5 0.250 0.250 0.500 126.4 17.5 '0.5 methanol'
6 0.250 0.750 0.000 126.4 17.5 '0.5 methanol'
7 0.500 0.276 0.250 36.1 2.5 ?
8 0.500 0.724 0.750 36.1 2.5 ?
9 0.500 0.215 0.750 23.1 0.9 ?
10 0.500 0.785 0.250 23.1 0.9 ?
11 0.750 0.250 0.000 126.4 17.5 '0.5 methanol'
12 0.750 0.750 0.500 126.4 17.5 '0.5 methanol'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_compound4
_database_code_depnum_ccdc_archive 'CCDC 2177799'
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_audit_creation_date             2021-11-15
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H102 N2 Ni2 O20 P4 Sb4, 2(C H4 O)'
_chemical_formula_sum            'C68 H110 N2 Ni2 O22 P4 Sb4'
_chemical_formula_weight         2035.87
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.249(3)
_cell_length_b                   20.009(3)
_cell_length_c                   16.163(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.427(2)
_cell_angle_gamma                90
_cell_volume                     8163.4(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5591
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.52
_shelx_estimated_absorpt_T_max   0.804
_shelx_estimated_absorpt_T_min   0.750
_exptl_absorpt_coefficient_mu    1.904
_exptl_absorpt_correction_T_max  0.8034
_exptl_absorpt_correction_T_min  0.7504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0595 before and 0.0335 after correction.
The Ratio of minimum to maximum transmission is 0.8291.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43172
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         1.299
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7315
_reflns_number_total             8334
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0365
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0419P)²+15.5094P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0873
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C16(H16)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C23(H23), C3(H3), C19(H19), C12(H12), C21(H21), C6(H6), C2(H2),
 C5(H5), C22(H22), C20(H20), C15(H15), C14(H14)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C27(H27A,H27B,
 H27C), C9(H9A,H9B,H9C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C25(H25A,
 H25B,H25C), C29(H29A,H29B,H29C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C34(H34A,H34B,H34C)
2.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Sb2 Sb 0.72665(2) 0.21716(2) 0.65092(2) 0.01856(7) Uani 1 1 d . . . . .
Sb1 Sb 0.65590(2) 0.30191(2) 0.47845(2) 0.01921(7) Uani 1 1 d . . . . .
Ni1 Ni 0.82410(2) 0.31729(2) 0.64598(3) 0.02015(11) Uani 1 1 d . . . . .
P1 P 0.76166(4) 0.39991(5) 0.49310(6) 0.0195(2) Uani 1 1 d . . . . .
P2 P 0.65747(4) 0.32195(5) 0.28338(6) 0.0213(2) Uani 1 1 d . . . . .
O2 O 0.67458(9) 0.26478(13) 0.58479(14) 0.0204(5) Uani 1 1 d . . . . .
O9 O 0.71816(9) 0.33553(13) 0.28019(15) 0.0212(5) Uani 1 1 d . . . . .
O3 O 0.71425(9) 0.25793(12) 0.42056(14) 0.0185(5) Uani 1 1 d . . . . .
O4 O 0.70192(9) 0.38236(12) 0.49990(15) 0.0206(5) Uani 1 1 d . . . . .
O5 O 0.75333(10) 0.30100(12) 0.70851(15) 0.0224(6) Uani 1 1 d . . . . .
O1 O 0.61904(10) 0.21775(13) 0.43519(15) 0.0227(6) Uani 1 1 d . . . . .
O8 O 0.63638(9) 0.34606(13) 0.36735(15) 0.0227(6) Uani 1 1 d . . . . .
O7 O 0.78525(9) 0.36582(12) 0.41628(15) 0.0211(5) Uani 1 1 d . . . . .
O10 O 0.64484(10) 0.24954(13) 0.26742(15) 0.0253(6) Uani 1 1 d . . . . .
O6 O 0.79323(10) 0.38745(13) 0.57075(15) 0.0229(6) Uani 1 1 d . . . . .
N1 N 0.86491(12) 0.39140(16) 0.71007(19) 0.0257(7) Uani 1 1 d . . . . .
C24 C 0.76323(15) 0.48825(18) 0.4699(2) 0.0239(8) Uani 1 1 d . . . . .
C10 C 0.67022(14) 0.19259(18) 0.7405(2) 0.0214(8) Uani 1 1 d . . . . .
C26 C 0.82171(16) 0.5100(2) 0.4675(3) 0.0329(9) Uani 1 1 d . . . . .
H26A H 0.838476 0.503759 0.522255 0.049 Uiso 1 1 calc GR . . . .
H26B H 0.823680 0.557167 0.451693 0.049 Uiso 1 1 calc GR . . . .
H26C H 0.840185 0.482745 0.426825 0.049 Uiso 1 1 calc GR . . . .
C1 C 0.58711(14) 0.34618(18) 0.5255(2) 0.0216(8) Uani 1 1 d . . . . .
C11 C 0.68431(16) 0.1671(2) 0.8172(2) 0.0314(9) Uani 1 1 d . . . . .
H11 H 0.720478 0.157489 0.829716 0.038 Uiso 1 1 calc R . . . .
C7 C 0.44575(16) 0.4365(2) 0.6207(3) 0.0319(9) Uani 1 1 d . . . . .
H7 H 0.456050 0.459946 0.673351 0.038 Uiso 1 1 calc R . . . .
C32 C 0.59180(16) 0.1738(2) 0.4886(2) 0.0294(9) Uani 1 1 d . . . . .
H32A H 0.617213 0.153080 0.527617 0.044 Uiso 1 1 calc GR . . . .
H32B H 0.573960 0.138930 0.455693 0.044 Uiso 1 1 calc GR . . . .
H32C H 0.565469 0.199019 0.519346 0.044 Uiso 1 1 calc GR . . . .
C31 C 0.64328(16) 0.3495(2) 0.1200(2) 0.0294(9) Uani 1 1 d . . . . .
H31A H 0.681874 0.352743 0.116268 0.044 Uiso 1 1 calc GR . . . .
H31B H 0.626410 0.376993 0.076700 0.044 Uiso 1 1 calc GR . . . .
H31C H 0.632375 0.302785 0.112667 0.044 Uiso 1 1 calc GR . . . .
O11 O 0.68477(17) 0.1735(2) 0.1241(3) 0.0659(11) Uani 1 1 d . . . . .
H11A H 0.676679 0.197420 0.164584 0.099 Uiso 1 1 calc GR . . . .
C23 C 0.84806(17) 0.4544(2) 0.7110(2) 0.0325(9) Uani 1 1 d . . . . .
H23 H 0.816128 0.465082 0.681636 0.039 Uiso 1 1 calc R . . . .
C28 C 0.62635(14) 0.3743(2) 0.2052(2) 0.0248(8) Uani 1 1 d . . . . .
C27 C 0.73612(17) 0.5009(2) 0.3855(3) 0.0334(10) Uani 1 1 d . . . . .
H27A H 0.755086 0.476731 0.342566 0.050 Uiso 1 1 calc GR . . . .
H27B H 0.736572 0.548883 0.373294 0.050 Uiso 1 1 calc GR . . . .
H27C H 0.699384 0.485199 0.386511 0.050 Uiso 1 1 calc GR . . . .
C3 C 0.54341(15) 0.4107(2) 0.6294(2) 0.0306(9) Uani 1 1 d . . . . .
H3 H 0.545591 0.435955 0.679104 0.037 Uiso 1 1 calc R . . . .
C4 C 0.49484(15) 0.4026(2) 0.5892(2) 0.0266(8) Uani 1 1 d . . . . .
C19 C 0.90931(17) 0.3777(2) 0.7528(3) 0.0377(10) Uani 1 1 d . . . . .
H19 H 0.921987 0.332978 0.753677 0.045 Uiso 1 1 calc R . . . .
C9 C 0.42531(17) 0.4889(2) 0.5605(3) 0.0349(10) Uani 1 1 d . . . . .
H9A H 0.452835 0.522576 0.552224 0.052 Uiso 1 1 calc GR . . . .
H9B H 0.393841 0.510331 0.582877 0.052 Uiso 1 1 calc GR . . . .
H9C H 0.416012 0.467666 0.507484 0.052 Uiso 1 1 calc GR . . . .
C13 C 0.59322(16) 0.1687(2) 0.8606(3) 0.0329(10) Uani 1 1 d . . . . .
C12 C 0.64644(17) 0.1552(2) 0.8766(3) 0.0373(11) Uani 1 1 d . . . . .
H12 H 0.657196 0.137519 0.928892 0.045 Uiso 1 1 calc R . . . .
C21 C 0.92032(19) 0.4901(3) 0.7959(3) 0.0439(12) Uani 1 1 d . . . . .
H21 H 0.939389 0.523962 0.825128 0.053 Uiso 1 1 calc R . . . .
C30 C 0.64279(16) 0.4476(2) 0.2171(2) 0.0313(9) Uani 1 1 d . . . . .
H30A H 0.630926 0.463475 0.270901 0.047 Uiso 1 1 calc GR . . . .
H30B H 0.626497 0.474823 0.172962 0.047 Uiso 1 1 calc GR . . . .
H30C H 0.681436 0.451238 0.214971 0.047 Uiso 1 1 calc GR . . . .
C6 C 0.53850(15) 0.3369(2) 0.4845(2) 0.0279(9) Uani 1 1 d . . . . .
H6 H 0.536482 0.311823 0.434674 0.033 Uiso 1 1 calc R . . . .
C33 C 0.71781(17) 0.3537(2) 0.7270(3) 0.0341(10) Uani 1 1 d . . . . .
H33A H 0.711255 0.380792 0.677265 0.051 Uiso 1 1 calc GR . . . .
H33B H 0.733383 0.381736 0.770905 0.051 Uiso 1 1 calc GR . . . .
H33C H 0.684286 0.334841 0.745451 0.051 Uiso 1 1 calc GR . . . .
C2 C 0.58932(15) 0.3822(2) 0.5981(2) 0.0302(9) Uani 1 1 d . . . . .
H2 H 0.622228 0.387746 0.627121 0.036 Uiso 1 1 calc R . . . .
C25 C 0.73494(17) 0.5270(2) 0.5372(3) 0.0339(10) Uani 1 1 d . . . . .
H25A H 0.697691 0.513350 0.537983 0.051 Uiso 1 1 calc GR . . . .
H25B H 0.737075 0.575019 0.525651 0.051 Uiso 1 1 calc GR . . . .
H25C H 0.751915 0.517594 0.591132 0.051 Uiso 1 1 calc GR . . . .
C5 C 0.49283(15) 0.3646(2) 0.5170(3) 0.0302(9) Uani 1 1 d . . . . .
H5 H 0.459686 0.357421 0.489296 0.036 Uiso 1 1 calc R . . . .
C29 C 0.56575(15) 0.3682(3) 0.2121(3) 0.0386(11) Uani 1 1 d . . . . .
H29A H 0.555172 0.321465 0.204029 0.058 Uiso 1 1 calc GR . . . .
H29B H 0.548335 0.396036 0.169600 0.058 Uiso 1 1 calc GR . . . .
H29C H 0.555208 0.383184 0.267002 0.058 Uiso 1 1 calc GR . . . .
C22 C 0.87455(19) 0.5048(2) 0.7525(3) 0.0422(11) Uani 1 1 d . . . . .
H22 H 0.861256 0.549172 0.750993 0.051 Uiso 1 1 calc R . . . .
C16 C 0.55118(17) 0.1557(3) 0.9245(3) 0.0405(11) Uani 1 1 d . . . . .
H16 H 0.517605 0.176826 0.903334 0.049 Uiso 1 1 calc R . . . .
C20 C 0.93769(18) 0.4260(3) 0.7959(3) 0.0459(12) Uani 1 1 d . . . . .
H20 H 0.969316 0.414353 0.825520 0.055 Uiso 1 1 calc R . . . .
C8 C 0.40272(18) 0.3864(2) 0.6409(3) 0.0462(12) Uani 1 1 d . . . . .
H8A H 0.390521 0.363966 0.590024 0.069 Uiso 1 1 calc GR . . . .
H8B H 0.372924 0.409759 0.665723 0.069 Uiso 1 1 calc GR . . . .
H8C H 0.416974 0.353143 0.680033 0.069 Uiso 1 1 calc GR . . . .
C15 C 0.61673(17) 0.2056(3) 0.7243(3) 0.0439(12) Uani 1 1 d . . . . .
H15 H 0.605746 0.222910 0.671902 0.053 Uiso 1 1 calc R . . . .
C14 C 0.57963(17) 0.1936(3) 0.7836(3) 0.0457(13) Uani 1 1 d . . . . .
H14 H 0.543431 0.202791 0.770922 0.055 Uiso 1 1 calc R . . . .
C17 C 0.5649(2) 0.1877(3) 1.0071(3) 0.0490(13) Uani 1 1 d . . . . .
H17A H 0.596311 0.165875 1.031647 0.073 Uiso 1 1 calc GR . . . .
H17B H 0.535070 0.182689 1.044214 0.073 Uiso 1 1 calc GR . . . .
H17C H 0.572300 0.235324 0.999002 0.073 Uiso 1 1 calc GR . . . .
C18 C 0.5405(2) 0.0812(3) 0.9336(4) 0.0694(18) Uani 1 1 d . . . . .
H18A H 0.529475 0.062605 0.879828 0.104 Uiso 1 1 calc GR . . . .
H18B H 0.512284 0.074432 0.973331 0.104 Uiso 1 1 calc GR . . . .
H18C H 0.572824 0.058743 0.953609 0.104 Uiso 1 1 calc GR . . . .
C34 C 0.7257(3) 0.2040(3) 0.0812(4) 0.0695(17) Uani 1 1 d . . . . .
H34A H 0.711442 0.241917 0.049393 0.104 Uiso 1 1 calc GR . . . .
H34B H 0.741294 0.171589 0.043487 0.104 Uiso 1 1 calc GR . . . .
H34C H 0.752909 0.219875 0.120758 0.104 Uiso 1 1 calc GR . . . .


_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
Sb2 O2 1.926(2) . ?
Sb2 O9 2.053(2) 7_656 ?
Sb2 O3 1.974(2) 7_656 ?
Sb2 O5 2.025(3) . ?
Sb2 O7 2.003(2) 7_656 ?
Sb2 C10 2.114(4) . ?
Sb1 O2 1.921(2) . ?
Sb1 O3 1.972(2) . ?
Sb1 O4 2.010(2) . ?
Sb1 O1 2.039(3) . ?
Sb1 O8 2.050(2) . ?
Sb1 C1 2.108(3) . ?
Ni1 O3 2.076(3) 7_656 ?
Ni1 O5 2.100(3) . ?
Ni1 O1 2.090(2) 7_656 ?
Ni1 O10 2.076(3) 7_656 ?
Ni1 O6 2.002(2) . ?
Ni1 N1 2.069(3) . ?
P1 O4 1.555(3) . ?
P1 O7 1.549(2) . ?
P1 O6 1.491(3) . ?
P1 C24 1.808(4) . ?
P2 O9 1.558(2) . ?
P2 O8 1.547(3) . ?
P2 O10 1.505(3) . ?
P2 C28 1.805(4) . ?
O5 C33 1.420(4) . ?
O1 C32 1.422(4) . ?
N1 C23 1.330(5) . ?
N1 C19 1.331(5) . ?
C24 C26 1.541(5) . ?
C24 C27 1.533(5) . ?
C24 C25 1.527(5) . ?
C10 C11 1.379(5) . ?
C10 C15 1.394(5) . ?
C1 C6 1.392(5) . ?
C1 C2 1.378(5) . ?
C11 C12 1.392(5) . ?
C7 C4 1.513(5) . ?
C7 C9 1.512(6) . ?
C7 C8 1.520(6) . ?
C31 C28 1.535(5) . ?
O11 C34 1.399(7) . ?
C23 C22 1.375(6) . ?
C28 C30 1.535(6) . ?
C28 C29 1.542(5) . ?
C3 C4 1.383(6) . ?
C3 C2 1.397(5) . ?
C4 C5 1.393(6) . ?
C19 C20 1.382(6) . ?
C13 C12 1.388(6) . ?
C13 C16 1.521(5) . ?
C13 C14 1.376(6) . ?
C21 C22 1.368(7) . ?
C21 C20 1.356(7) . ?
C6 C5 1.393(5) . ?
C16 C17 1.514(7) . ?
C16 C18 1.522(7) . ?
C15 C14 1.378(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
O2 Sb2 O9 178.68(11) . 7_656 ?
O2 Sb2 O3 93.78(10) . 7_656 ?
O2 Sb2 O5 93.44(10) . . ?
O2 Sb2 O7 91.03(11) . 7_656 ?
O2 Sb2 C10 91.86(12) . . ?
O9 Sb2 C10 88.23(12) 7_656 . ?
O3 Sb2 O9 86.24(9) 7_656 7_656 ?
O3 Sb2 O5 79.18(10) 7_656 . ?
O3 Sb2 O7 89.84(10) 7_656 7_656 ?
O3 Sb2 C10 172.63(12) 7_656 . ?
O5 Sb2 O9 87.87(10) . 7_656 ?
O5 Sb2 C10 95.75(12) . . ?
O7 Sb2 O9 87.65(10) 7_656 7_656 ?
O7 Sb2 O5 168.39(10) 7_656 . ?
O7 Sb2 C10 94.81(12) 7_656 . ?
O2 Sb1 O3 94.72(10) . . ?
O2 Sb1 O4 91.57(10) . . ?
O2 Sb1 O1 95.00(11) . . ?
O2 Sb1 O8 177.23(11) . . ?
O2 Sb1 C1 91.48(12) . . ?
O3 Sb1 O4 90.21(10) . . ?
O3 Sb1 O1 78.98(10) . . ?
O3 Sb1 O8 86.72(10) . . ?
O3 Sb1 C1 172.09(12) . . ?
O4 Sb1 O1 167.76(10) . . ?
O4 Sb1 O8 86.06(10) . . ?
O4 Sb1 C1 94.54(12) . . ?
O1 Sb1 O8 87.59(10) . . ?
O1 Sb1 C1 95.60(13) . . ?
O8 Sb1 C1 87.29(12) . . ?
O3 Ni1 O5 75.24(9) 7_656 . ?
O3 Ni1 O1 75.54(9) 7_656 7_656 ?
O3 Ni1 O10 92.63(10) 7_656 7_656 ?
O1 Ni1 O5 148.87(10) 7_656 . ?
O10 Ni1 O5 83.52(10) 7_656 . ?
O10 Ni1 O1 87.32(10) 7_656 7_656 ?
O6 Ni1 O3 91.39(10) . 7_656 ?
O6 Ni1 O5 94.47(10) . . ?
O6 Ni1 O1 96.73(10) . 7_656 ?
O6 Ni1 O10 174.90(10) . 7_656 ?
O6 Ni1 N1 89.03(11) . . ?
N1 Ni1 O3 177.87(11) . 7_656 ?
N1 Ni1 O5 106.82(11) . . ?
N1 Ni1 O1 102.33(11) . 7_656 ?
N1 Ni1 O10 87.08(12) . 7_656 ?
O4 P1 C24 105.18(16) . . ?
O7 P1 O4 110.50(14) . . ?
O7 P1 C24 104.70(16) . . ?
O6 P1 O4 113.70(14) . . ?
O6 P1 O7 113.15(14) . . ?
O6 P1 C24 108.89(17) . . ?
O9 P2 C28 106.67(16) . . ?
O8 P2 O9 109.56(14) . . ?
O8 P2 C28 106.24(16) . . ?
O10 P2 O9 111.51(15) . . ?
O10 P2 O8 112.00(15) . . ?
O10 P2 C28 110.58(17) . . ?
Sb1 O2 Sb2 146.83(13) . . ?
P2 O9 Sb2 123.17(14) . 7_656 ?
Sb2 O3 Ni1 103.27(10) 7_656 7_656 ?
Sb1 O3 Sb2 138.56(13) . 7_656 ?
Sb1 O3 Ni1 103.00(10) . 7_656 ?
P1 O4 Sb1 136.55(15) . . ?
Sb2 O5 Ni1 100.64(10) . . ?
C33 O5 Sb2 120.4(2) . . ?
C33 O5 Ni1 122.4(2) . . ?
Sb1 O1 Ni1 100.23(11) . 7_656 ?
C32 O1 Sb1 121.8(2) . . ?
C32 O1 Ni1 121.6(2) . 7_656 ?
P2 O8 Sb1 123.60(14) . . ?
P1 O7 Sb2 138.10(15) . 7_656 ?
P2 O10 Ni1 115.46(15) . 7_656 ?
P1 O6 Ni1 145.11(17) . . ?
C23 N1 Ni1 122.0(3) . . ?
C19 N1 Ni1 121.0(3) . . ?
C19 N1 C23 117.1(4) . . ?
C26 C24 P1 107.9(3) . . ?
C27 C24 P1 109.5(3) . . ?
C27 C24 C26 109.7(3) . . ?
C25 C24 P1 109.7(3) . . ?
C25 C24 C26 109.9(3) . . ?
C25 C24 C27 110.1(3) . . ?
C11 C10 Sb2 122.6(3) . . ?
C11 C10 C15 117.7(4) . . ?
C15 C10 Sb2 119.6(3) . . ?
C6 C1 Sb1 119.8(3) . . ?
C2 C1 Sb1 120.7(3) . . ?
C2 C1 C6 119.4(3) . . ?
C10 C11 C12 121.1(4) . . ?
C4 C7 C8 111.9(4) . . ?
C9 C7 C4 111.3(3) . . ?
C9 C7 C8 111.2(4) . . ?
N1 C23 C22 123.3(4) . . ?
C31 C28 P2 108.3(3) . . ?
C31 C28 C30 109.9(3) . . ?
C31 C28 C29 109.8(3) . . ?
C30 C28 P2 110.8(3) . . ?
C30 C28 C29 109.4(3) . . ?
C29 C28 P2 108.6(3) . . ?
C4 C3 C2 121.1(4) . . ?
C3 C4 C7 120.9(4) . . ?
C3 C4 C5 118.1(3) . . ?
C5 C4 C7 121.0(4) . . ?
N1 C19 C20 122.5(4) . . ?
C12 C13 C16 122.0(4) . . ?
C14 C13 C12 117.2(4) . . ?
C14 C13 C16 120.9(4) . . ?
C13 C12 C11 121.1(4) . . ?
C20 C21 C22 118.1(4) . . ?
C1 C6 C5 119.8(4) . . ?
C1 C2 C3 120.3(4) . . ?
C4 C5 C6 121.3(4) . . ?
C21 C22 C23 119.2(5) . . ?
C13 C16 C18 111.2(4) . . ?
C17 C16 C13 112.2(4) . . ?
C17 C16 C18 111.5(4) . . ?
C21 C20 C19 119.9(5) . . ?
C14 C15 C10 120.6(4) . . ?
C13 C14 C15 122.3(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_compound2
_database_code_depnum_ccdc_archive 'CCDC 2177797'
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_audit_creation_date             2021-11-15
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C66 H102 Mn2 N2 O20 P4 Sb4, 2(C H4 O)'
_chemical_formula_sum            'C68 H110 Mn2 N2 O22 P4 Sb4'
_chemical_formula_weight         2028.33
_chemical_melting_point          ?
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'
Mn Mn 0.3368 0.7283 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.252(3)
_cell_length_b                   20.379(3)
_cell_length_c                   16.0757(18)
_cell_angle_alpha                90
_cell_angle_beta                 91.123(2)
_cell_angle_gamma                90
_cell_volume                     8271.1(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9185
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.37
_shelx_estimated_absorpt_T_max   0.806
_shelx_estimated_absorpt_T_min   0.769
_exptl_absorpt_coefficient_mu    1.730
_exptl_absorpt_correction_T_max  0.8064
_exptl_absorpt_correction_T_min  0.7693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS v 2.10 (Bruker, 2003) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43796
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_min         1.284
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7761
_reflns_number_total             8474
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8474
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0356
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0363P)²+30.0788P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0837
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C16(H16), C7(H7)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C11(H11), C12(H12), C15(H15), C6(H6), C23(H23), C5(H5), C2(H2),
 C3(H3), C19(H19), C22(H22), C21(H21), C20(H20)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C27(H27A,H27B,
 H27C), C33(H33A,H33B,H33C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C26(H26A,
 H26B,H26C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C9(H9A,H9B,H9C), C8(H8A,
 H8B,H8C), C34(H34A,H34B,H34C)
2.d Idealised tetrahedral OH refined as rotating group:
 O11(H11A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Sb2 Sb 0.65665(2) 0.80238(2) 0.47934(2) 0.01521(7) Uani 1 1 d . . . . .
Sb1 Sb 0.72651(2) 0.71670(2) 0.65088(2) 0.01504(7) Uani 1 1 d . . . . .
Mn1 Mn 0.67405(2) 0.67681(3) 0.35109(3) 0.01857(12) Uani 1 1 d . . . . .
P1 P 0.84319(3) 0.67984(5) 0.71855(6) 0.01823(19) Uani 1 1 d . . . . .
P2 P 0.73858(3) 0.59861(4) 0.50863(6) 0.01699(18) Uani 1 1 d . . . . .
O5 O 0.67456(9) 0.76498(12) 0.58627(14) 0.0175(5) Uani 1 1 d . . . . .
O1 O 0.61860(9) 0.72041(12) 0.43972(15) 0.0192(5) Uani 1 1 d . . . . .
O7 O 0.78239(9) 0.66721(12) 0.72126(15) 0.0189(5) Uani 1 1 d . . . . .
O6 O 0.75123(9) 0.79878(12) 0.70971(15) 0.0197(5) Uani 1 1 d . . . . .
O4 O 0.71393(9) 0.63482(12) 0.58365(15) 0.0184(5) Uani 1 1 d . . . . .
O8 O 0.79744(9) 0.61816(12) 0.49945(15) 0.0195(5) Uani 1 1 d . . . . .
O2 O 0.71483(8) 0.75939(12) 0.42137(14) 0.0167(5) Uani 1 1 d . . . . .
O9 O 0.86413(9) 0.65678(12) 0.63339(15) 0.0195(5) Uani 1 1 d . . . . .
O10 O 0.85688(9) 0.75039(13) 0.73668(15) 0.0221(5) Uani 1 1 d . . . . .
O3 O 0.70670(9) 0.60671(12) 0.42981(15) 0.0222(5) Uani 1 1 d . . . . .
N1 N 0.62850(14) 0.60037(17) 0.2822(2) 0.0321(8) Uani 1 1 d . . . . .
C1 C 0.66998(14) 0.69091(17) 0.7401(2) 0.0197(7) Uani 1 1 d . . . . .
C10 C 0.58877(13) 0.84790(17) 0.5267(2) 0.0179(7) Uani 1 1 d . . . . .
C16 C 0.44769(14) 0.93916(19) 0.6235(2) 0.0248(8) Uani 1 1 d . . . . .
H16 H 0.458279 0.963256 0.675375 0.030 Uiso 1 1 calc R . . . .
C24 C 0.73814(14) 0.51277(17) 0.5368(2) 0.0221(8) Uani 1 1 d . . . . .
C13 C 0.49664(14) 0.90544(18) 0.5910(2) 0.0221(8) Uani 1 1 d . . . . .
C25 C 0.68039(15) 0.49022(19) 0.5430(3) 0.0298(9) Uani 1 1 d . . . . .
H25A H 0.662050 0.517811 0.583189 0.045 Uiso 1 1 calc GR . . . .
H25B H 0.679474 0.444395 0.561378 0.045 Uiso 1 1 calc GR . . . .
H25C H 0.662766 0.494044 0.488337 0.045 Uiso 1 1 calc GR . . . .
C28 C 0.87378(14) 0.62698(19) 0.7968(2) 0.0225(8) Uani 1 1 d . . . . .
C14 C 0.54588(15) 0.9144(2) 0.6295(2) 0.0266(8) Uani 1 1 d . . . . .
H14 H 0.548502 0.940676 0.678254 0.032 Uiso 1 1 calc R . . . .
C31 C 0.85651(15) 0.6509(2) 0.8826(2) 0.0273(8) Uani 1 1 d . . . . .
H31A H 0.868583 0.696168 0.891277 0.041 Uiso 1 1 calc GR . . . .
H31B H 0.872109 0.622641 0.925903 0.041 Uiso 1 1 calc GR . . . .
H31C H 0.817802 0.649283 0.885562 0.041 Uiso 1 1 calc GR . . . .
O11 O 0.81734(19) 0.8252(2) 0.8767(3) 0.0717(12) Uani 1 1 d . . . . .
H11A H 0.821742 0.805200 0.831634 0.108 Uiso 1 1 calc GR . . . .
C11 C 0.53955(14) 0.83793(19) 0.4876(2) 0.0250(8) Uani 1 1 d . . . . .
H11 H 0.537048 0.811720 0.438855 0.030 Uiso 1 1 calc R . . . .
C12 C 0.49411(14) 0.86617(19) 0.5198(2) 0.0259(8) Uani 1 1 d . . . . .
H12 H 0.460835 0.858612 0.492923 0.031 Uiso 1 1 calc R . . . .
C15 C 0.59157(14) 0.88576(19) 0.5981(2) 0.0247(8) Uani 1 1 d . . . . .
H15 H 0.624697 0.892257 0.625941 0.030 Uiso 1 1 calc R . . . .
C29 C 0.85669(16) 0.55540(19) 0.7840(2) 0.0294(9) Uani 1 1 d . . . . .
H29A H 0.817991 0.552422 0.785568 0.044 Uiso 1 1 calc GR . . . .
H29B H 0.872310 0.528128 0.828279 0.044 Uiso 1 1 calc GR . . . .
H29C H 0.868863 0.539917 0.729900 0.044 Uiso 1 1 calc GR . . . .
C27 C 0.76661(16) 0.5038(2) 0.6211(3) 0.0316(9) Uani 1 1 d . . . . .
H27A H 0.802762 0.520973 0.618037 0.047 Uiso 1 1 calc GR . . . .
H27B H 0.767866 0.457023 0.635255 0.047 Uiso 1 1 calc GR . . . .
H27C H 0.747389 0.527624 0.664046 0.047 Uiso 1 1 calc GR . . . .
C33 C 0.59042(15) 0.6796(2) 0.4959(3) 0.0280(9) Uani 1 1 d . . . . .
H33A H 0.615703 0.655522 0.531420 0.042 Uiso 1 1 calc GR . . . .
H33B H 0.568407 0.648468 0.464289 0.042 Uiso 1 1 calc GR . . . .
H33C H 0.567814 0.706968 0.530676 0.042 Uiso 1 1 calc GR . . . .
C6 C 0.68385(16) 0.6621(2) 0.8159(3) 0.0343(10) Uani 1 1 d . . . . .
H6 H 0.719697 0.650178 0.826828 0.041 Uiso 1 1 calc R . . . .
C17 C 0.42677(16) 0.9894(2) 0.5611(3) 0.0317(9) Uani 1 1 d . . . . .
H17A H 0.454711 1.021147 0.549064 0.048 Uiso 1 1 calc GR . . . .
H17B H 0.396362 1.012298 0.584513 0.048 Uiso 1 1 calc GR . . . .
H17C H 0.415744 0.967029 0.509676 0.048 Uiso 1 1 calc GR . . . .
C4 C 0.59325(15) 0.6667(2) 0.8629(3) 0.0317(9) Uani 1 1 d . . . . .
C18 C 0.40482(16) 0.8901(2) 0.6461(3) 0.0361(10) Uani 1 1 d . . . . .
H18A H 0.393165 0.866225 0.596018 0.054 Uiso 1 1 calc GR . . . .
H18B H 0.374660 0.913455 0.669482 0.054 Uiso 1 1 calc GR . . . .
H18C H 0.419057 0.858911 0.687207 0.054 Uiso 1 1 calc GR . . . .
C7 C 0.55142(17) 0.6548(3) 0.9281(3) 0.0406(11) Uani 1 1 d . . . . .
H7 H 0.516953 0.671617 0.905081 0.049 Uiso 1 1 calc R . . . .
C26 C 0.76655(17) 0.47361(19) 0.4696(3) 0.0339(10) Uani 1 1 d . . . . .
H26A H 0.748102 0.479637 0.415989 0.051 Uiso 1 1 calc GR . . . .
H26B H 0.766612 0.426952 0.484415 0.051 Uiso 1 1 calc GR . . . .
H26C H 0.803131 0.489179 0.465588 0.051 Uiso 1 1 calc GR . . . .
C32 C 0.71465(17) 0.8475(2) 0.7342(3) 0.0375(10) Uani 1 1 d . . . . .
H32A H 0.711556 0.881029 0.690703 0.056 Uiso 1 1 calc GR . . . .
H32B H 0.727149 0.867875 0.786222 0.056 Uiso 1 1 calc GR . . . .
H32C H 0.679963 0.827279 0.742697 0.056 Uiso 1 1 calc GR . . . .
C23 C 0.64018(19) 0.5365(2) 0.2885(3) 0.0369(10) Uani 1 1 d . . . . .
H23 H 0.669313 0.524080 0.323383 0.044 Uiso 1 1 calc R . . . .
C30 C 0.93401(14) 0.6328(2) 0.7897(3) 0.0368(11) Uani 1 1 d . . . . .
H30A H 0.944623 0.617704 0.734548 0.055 Uiso 1 1 calc GR . . . .
H30B H 0.951318 0.605623 0.832555 0.055 Uiso 1 1 calc GR . . . .
H30C H 0.944623 0.678657 0.797313 0.055 Uiso 1 1 calc GR . . . .
C5 C 0.64603(17) 0.6503(2) 0.8761(3) 0.0405(11) Uani 1 1 d . . . . .
H5 H 0.656647 0.630562 0.927276 0.049 Uiso 1 1 calc R . . . .
C2 C 0.61711(16) 0.7084(2) 0.7282(3) 0.0355(10) Uani 1 1 d . . . . .
H2 H 0.606400 0.729166 0.677728 0.043 Uiso 1 1 calc R . . . .
C3 C 0.57989(16) 0.6963(2) 0.7879(3) 0.0399(11) Uani 1 1 d . . . . .
H3 H 0.544099 0.708526 0.777285 0.048 Uiso 1 1 calc R . . . .
C9 C 0.5638(2) 0.6925(3) 1.0076(3) 0.0480(12) Uani 1 1 d . . . . .
H9A H 0.595885 0.674544 1.034235 0.072 Uiso 1 1 calc GR . . . .
H9B H 0.534060 0.688379 1.045555 0.072 Uiso 1 1 calc GR . . . .
H9C H 0.569382 0.738874 0.994342 0.072 Uiso 1 1 calc GR . . . .
C19 C 0.58674(19) 0.6158(3) 0.2326(3) 0.0470(12) Uani 1 1 d . . . . .
H19 H 0.577241 0.660721 0.226968 0.056 Uiso 1 1 calc R . . . .
C22 C 0.6124(2) 0.4875(3) 0.2474(3) 0.0509(13) Uani 1 1 d . . . . .
H22 H 0.622355 0.442786 0.254094 0.061 Uiso 1 1 calc R . . . .
C21 C 0.5700(2) 0.5045(3) 0.1965(3) 0.0523(13) Uani 1 1 d . . . . .
H21 H 0.550261 0.472020 0.167013 0.063 Uiso 1 1 calc R . . . .
C8 C 0.5445(2) 0.5819(3) 0.9454(3) 0.0552(14) Uani 1 1 d . . . . .
H8A H 0.535487 0.559020 0.893407 0.083 Uiso 1 1 calc GR . . . .
H8B H 0.515974 0.575681 0.985137 0.083 Uiso 1 1 calc GR . . . .
H8C H 0.577578 0.563982 0.968872 0.083 Uiso 1 1 calc GR . . . .
C20 C 0.5571(2) 0.5696(3) 0.1896(3) 0.0537(14) Uani 1 1 d . . . . .
H20 H 0.527878 0.582909 0.155494 0.064 Uiso 1 1 calc R . . . .
C34 C 0.7766(3) 0.7937(3) 0.9222(4) 0.0738(19) Uani 1 1 d . . . . .
H34A H 0.752785 0.770351 0.883495 0.111 Uiso 1 1 calc GR . . . .
H34B H 0.756569 0.826669 0.952733 0.111 Uiso 1 1 calc GR . . . .
H34C H 0.792583 0.762331 0.961534 0.111 Uiso 1 1 calc GR . . . .


_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
Sb2 O5 1.926(2) . ?
Sb2 O1 2.024(2) . ?
Sb2 O8 2.017(2) 7_666 ?
Sb2 O2 1.962(2) . ?
Sb2 O9 2.053(2) 7_666 ?
Sb2 C10 2.104(3) . ?
Sb1 O5 1.927(2) . ?
Sb1 O7 2.056(2) . ?
Sb1 O6 2.015(2) . ?
Sb1 O4 2.010(2) . ?
Sb1 O2 1.962(2) 7_666 ?
Sb1 C1 2.110(3) . ?
Mn1 O1 2.204(2) . ?
Mn1 O6 2.199(2) 7_666 ?
Mn1 O2 2.264(2) . ?
Mn1 O10 2.181(3) 7_666 ?
Mn1 O3 2.069(3) . ?
Mn1 N1 2.219(3) . ?
P1 O7 1.558(2) . ?
P1 O9 1.550(3) . ?
P1 O10 1.506(3) . ?
P1 C28 1.817(4) . ?
P2 O4 1.554(2) . ?
P2 O8 1.549(2) . ?
P2 O3 1.497(3) . ?
P2 C24 1.807(4) . ?
O1 C33 1.428(4) . ?
O6 C32 1.417(5) . ?
N1 C23 1.339(6) . ?
N1 C19 1.347(6) . ?
C1 C6 1.391(5) . ?
C1 C2 1.391(5) . ?
C10 C11 1.396(5) . ?
C10 C15 1.384(5) . ?
C16 C13 1.516(5) . ?
C16 C17 1.520(5) . ?
C16 C18 1.523(5) . ?
C24 C25 1.534(5) . ?
C24 C27 1.534(5) . ?
C24 C26 1.532(5) . ?
C13 C14 1.390(5) . ?
C13 C12 1.397(5) . ?
C28 C31 1.535(5) . ?
C28 C29 1.534(6) . ?
C28 C30 1.532(5) . ?
C14 C15 1.396(5) . ?
O11 C34 1.425(8) . ?
C11 C12 1.392(5) . ?
C6 C5 1.393(6) . ?
C4 C7 1.523(6) . ?
C4 C5 1.386(6) . ?
C4 C3 1.383(6) . ?
C7 C9 1.519(7) . ?
C7 C8 1.522(7) . ?
C23 C22 1.381(6) . ?
C2 C3 1.379(6) . ?
C19 C20 1.380(7) . ?
C22 C21 1.380(7) . ?
C21 C20 1.370(8) . ?

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
O5 Sb2 O1 93.21(10) . . ?
O5 Sb2 O8 92.44(10) . 7_666 ?
O5 Sb2 O2 94.72(9) . . ?
O5 Sb2 O9 178.57(9) . 7_666 ?
O5 Sb2 C10 91.74(11) . . ?
O1 Sb2 O9 86.86(10) . 7_666 ?
O1 Sb2 C10 95.32(12) . . ?
O8 Sb2 O1 169.68(10) 7_666 . ?
O8 Sb2 O9 87.70(10) 7_666 7_666 ?
O8 Sb2 C10 93.13(12) 7_666 . ?
O2 Sb2 O1 80.63(10) . . ?
O2 Sb2 O8 90.31(10) . 7_666 ?
O2 Sb2 O9 86.71(9) . 7_666 ?
O2 Sb2 C10 172.55(12) . . ?
O9 Sb2 C10 86.83(11) 7_666 . ?
O5 Sb1 O7 178.64(10) . . ?
O5 Sb1 O6 91.74(10) . . ?
O5 Sb1 O4 92.02(10) . . ?
O5 Sb1 O2 93.90(10) . 7_666 ?
O5 Sb1 C1 91.79(12) . . ?
O7 Sb1 C1 88.26(12) . . ?
O6 Sb1 O7 86.90(10) . . ?
O6 Sb1 C1 95.45(12) . . ?
O4 Sb1 O7 89.33(10) . . ?
O4 Sb1 O6 170.39(9) . . ?
O4 Sb1 C1 93.27(12) . . ?
O2 Sb1 O7 85.96(9) 7_666 . ?
O2 Sb1 O6 80.86(10) 7_666 . ?
O2 Sb1 O4 90.06(10) 7_666 . ?
O2 Sb1 C1 173.30(12) 7_666 . ?
O1 Mn1 O2 70.50(8) . . ?
O1 Mn1 N1 106.01(12) . . ?
O6 Mn1 O1 139.26(9) 7_666 . ?
O6 Mn1 O2 70.60(9) 7_666 . ?
O6 Mn1 N1 112.20(12) 7_666 . ?
O10 Mn1 O1 85.41(9) 7_666 . ?
O10 Mn1 O6 81.84(9) 7_666 7_666 ?
O10 Mn1 O2 88.32(9) 7_666 . ?
O10 Mn1 N1 88.81(11) 7_666 . ?
O3 Mn1 O1 97.67(10) . . ?
O3 Mn1 O6 95.34(9) . 7_666 ?
O3 Mn1 O2 92.07(9) . . ?
O3 Mn1 O10 176.85(10) . 7_666 ?
O3 Mn1 N1 90.97(11) . . ?
N1 Mn1 O2 175.65(11) . . ?
O7 P1 C28 106.76(15) . . ?
O9 P1 O7 109.16(14) . . ?
O9 P1 C28 106.50(15) . . ?
O10 P1 O7 112.01(14) . . ?
O10 P1 O9 112.30(14) . . ?
O10 P1 C28 109.82(16) . . ?
O4 P2 C24 105.13(15) . . ?
O8 P2 O4 110.58(13) . . ?
O8 P2 C24 106.47(15) . . ?
O3 P2 O4 112.80(14) . . ?
O3 P2 O8 113.10(14) . . ?
O3 P2 C24 108.21(16) . . ?
Sb2 O5 Sb1 145.94(13) . . ?
Sb2 O1 Mn1 103.44(10) . . ?
C33 O1 Sb2 121.4(2) . . ?
C33 O1 Mn1 120.4(2) . . ?
P1 O7 Sb1 124.73(14) . . ?
Sb1 O6 Mn1 103.87(10) . 7_666 ?
C32 O6 Sb1 121.0(2) . . ?
C32 O6 Mn1 122.3(2) . 7_666 ?
P2 O4 Sb1 138.57(14) . . ?
P2 O8 Sb2 137.75(14) . 7_666 ?
Sb2 O2 Sb1 138.73(13) . 7_666 ?
Sb2 O2 Mn1 103.39(9) . . ?
Sb1 O2 Mn1 103.33(10) 7_666 . ?
P1 O9 Sb2 124.81(14) . 7_666 ?
P1 O10 Mn1 116.50(14) . 7_666 ?
P2 O3 Mn1 142.66(16) . . ?
C23 N1 Mn1 122.3(3) . . ?
C23 N1 C19 116.2(4) . . ?
C19 N1 Mn1 121.6(3) . . ?
C6 C1 Sb1 122.6(3) . . ?
C6 C1 C2 117.0(3) . . ?
C2 C1 Sb1 120.2(3) . . ?
C11 C10 Sb2 119.8(3) . . ?
C15 C10 Sb2 121.1(3) . . ?
C15 C10 C11 119.0(3) . . ?
C13 C16 C17 110.7(3) . . ?
C13 C16 C18 111.9(3) . . ?
C17 C16 C18 111.1(3) . . ?
C25 C24 P2 108.5(2) . . ?
C25 C24 C27 109.6(3) . . ?
C27 C24 P2 109.4(3) . . ?
C26 C24 P2 108.8(3) . . ?
C26 C24 C25 110.4(3) . . ?
C26 C24 C27 110.0(3) . . ?
C14 C13 C16 121.0(3) . . ?
C14 C13 C12 117.8(3) . . ?
C12 C13 C16 121.1(3) . . ?
C31 C28 P1 108.0(3) . . ?
C29 C28 P1 110.8(3) . . ?
C29 C28 C31 109.8(3) . . ?
C30 C28 P1 108.1(3) . . ?
C30 C28 C31 110.1(3) . . ?
C30 C28 C29 109.9(3) . . ?
C13 C14 C15 121.5(4) . . ?
C12 C11 C10 120.4(4) . . ?
C11 C12 C13 121.1(3) . . ?
C10 C15 C14 120.3(3) . . ?
C1 C6 C5 121.1(4) . . ?
C5 C4 C7 122.3(4) . . ?
C3 C4 C7 120.6(4) . . ?
C3 C4 C5 117.1(4) . . ?
C9 C7 C4 111.4(4) . . ?
C9 C7 C8 111.3(4) . . ?
C8 C7 C4 111.4(4) . . ?
N1 C23 C22 123.9(4) . . ?
C4 C5 C6 121.5(4) . . ?
C3 C2 C1 121.6(4) . . ?
C2 C3 C4 121.8(4) . . ?
N1 C19 C20 123.2(5) . . ?
C21 C22 C23 118.9(5) . . ?
C20 C21 C22 118.2(5) . . ?
C21 C20 C19 119.6(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
