# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2023174'
loop_
_audit_author_name
_audit_author_address
'Yile Wu'
;Ningbo University
China
;
_audit_update_record             
;
2020-08-13 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_audit_creation_date             2020-08-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C32 H42 Cl8 Ni2 O14 P2'
_chemical_formula_sum            'C32 H42 Cl8 Ni2 O14 P2'
_chemical_formula_weight         1113.61
_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 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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                   8.9110(5)
_cell_length_b                   11.1675(6)
_cell_length_c                   11.8597(7)
_cell_angle_alpha                108.4832(15)
_cell_angle_beta                 97.6582(16)
_cell_angle_gamma                100.3215(15)
_cell_volume                     1078.12(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      73.47
_cell_measurement_theta_min      4.30
_shelx_estimated_absorpt_T_max   0.387
_shelx_estimated_absorpt_T_min   0.370
_exptl_absorpt_coefficient_mu    6.897
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5410
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1120 before and 0.0906 after correction.
The Ratio of minimum to maximum transmission is 0.7179.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32977
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.465
_diffrn_reflns_theta_min         4.014
_diffrn_ambient_temperature      103.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4183
_reflns_number_total             4260
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4260
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0325
_refine_ls_restrained_S_all      1.060
_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+1.0232P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0856
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C14(H14A,H14B), C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Ni1 Ni 0.11984(4) 0.43620(3) 0.54300(3) 0.02123(10) Uani 1 1 d . . . . .
P2 P -0.18178(5) 0.42566(5) 0.63795(4) 0.02066(12) Uani 1 1 d . . . . .
Cl3 Cl -0.08812(6) 0.68852(5) 1.02204(4) 0.03252(13) Uani 1 1 d . . . . .
Cl4 Cl 0.27039(6) 0.85314(5) 0.65979(5) 0.03481(14) Uani 1 1 d . . . . .
Cl5 Cl 0.32060(7) 1.04568(5) 0.92678(6) 0.04200(15) Uani 1 1 d . . . . .
Cl6 Cl 0.14239(7) 0.96275(5) 1.10986(5) 0.03604(14) Uani 1 1 d . . . . .
O1 O 0.04925(16) 0.60573(13) 0.60743(12) 0.0225(3) Uani 1 1 d . . . . .
O2 O -0.04998(15) 0.36067(13) 0.61851(13) 0.0241(3) Uani 1 1 d . . . . .
O3 O 0.25854(15) 0.52793(13) 0.45488(13) 0.0236(3) Uani 1 1 d . . . . .
O4 O 0.17848(18) 0.26211(14) 0.47054(15) 0.0306(3) Uani 1 1 d . . . . .
O5 O 0.29214(17) 0.48305(16) 0.69472(14) 0.0318(3) Uani 1 1 d . . . . .
O6 O -0.12963(17) 0.54244(14) 0.76976(13) 0.0267(3) Uani 1 1 d . . . . .
O7 O -0.31768(15) 0.33659(13) 0.66830(13) 0.0241(3) Uani 1 1 d . . . . .
C8 C -0.0184(2) 0.65550(19) 0.80207(18) 0.0229(4) Uani 1 1 d . . . . .
C9 C -0.2816(2) 0.2778(2) 0.7587(2) 0.0289(4) Uani 1 1 d . . . . .
H9A H -0.2323 0.3461 0.8384 0.035 Uiso 1 1 calc R . . . .
H9B H -0.2086 0.2218 0.7345 0.035 Uiso 1 1 calc R . . . .
C10 C 0.0662(2) 0.68757(18) 0.71881(18) 0.0220(4) Uani 1 1 d . . . . .
C11 C 0.1146(2) 0.8586(2) 0.96180(18) 0.0269(4) Uani 1 1 d . . . . .
C12 C 0.1943(2) 0.8952(2) 0.8802(2) 0.0284(4) Uani 1 1 d . . . . .
C13 C 0.0086(2) 0.7381(2) 0.92210(18) 0.0249(4) Uani 1 1 d . . . . .
C14 C 0.4394(2) 0.5735(2) 0.7114(2) 0.0326(5) Uani 1 1 d . . . . .
H14A H 0.4217 0.6517 0.6943 0.039 Uiso 1 1 calc R . . . .
H14B H 0.5047 0.5322 0.6566 0.039 Uiso 1 1 calc R . . . .
C15 C 0.3527(3) 0.1256(2) 0.4188(2) 0.0345(5) Uani 1 1 d . . . . .
H15A H 0.4447 0.1420 0.4833 0.041 Uiso 1 1 calc R . . . .
H15B H 0.3734 0.0755 0.3396 0.041 Uiso 1 1 calc R . . . .
C16 C 0.1703(2) 0.8105(2) 0.76121(19) 0.0261(4) Uani 1 1 d . . . . .
C17 C -0.4316(3) 0.1985(2) 0.7673(2) 0.0349(5) Uani 1 1 d . . . . .
H17A H -0.4796 0.1315 0.6879 0.052 Uiso 1 1 calc GR . . . .
H17B H -0.5026 0.2550 0.7922 0.052 Uiso 1 1 calc GR . . . .
H17C H -0.4106 0.1571 0.8273 0.052 Uiso 1 1 calc GR . . . .
C18 C 0.2069(3) 0.0536(2) 0.4449(3) 0.0427(6) Uani 1 1 d . . . . .
H18A H 0.1299 0.0014 0.3690 0.051 Uiso 1 1 calc R . . . .
H18B H 0.2325 -0.0042 0.4892 0.051 Uiso 1 1 calc R . . . .
C19 C 0.2697(3) 0.4724(3) 0.8099(2) 0.0353(5) Uani 1 1 d . . . . .
H19A H 0.2949 0.3921 0.8173 0.042 Uiso 1 1 calc R . . . .
H19B H 0.1607 0.4715 0.8189 0.042 Uiso 1 1 calc R . . . .
C20 C 0.3806(3) 0.5914(3) 0.9041(2) 0.0491(7) Uani 1 1 d . . . . .
H20A H 0.4119 0.5763 0.9807 0.059 Uiso 1 1 calc R . . . .
H20B H 0.3339 0.6677 0.9212 0.059 Uiso 1 1 calc R . . . .
C21 C 0.5172(3) 0.6092(3) 0.8427(2) 0.0483(6) Uani 1 1 d . . . . .
H21A H 0.5792 0.7002 0.8764 0.058 Uiso 1 1 calc R . . . .
H21B H 0.5858 0.5508 0.8518 0.058 Uiso 1 1 calc R . . . .
C23 C 0.3143(3) 0.2523(2) 0.4169(2) 0.0364(5) Uani 1 1 d . . . . .
H23A H 0.4027 0.3268 0.4645 0.044 Uiso 1 1 calc R . . . .
H23B H 0.2918 0.2513 0.3325 0.044 Uiso 1 1 calc R . . . .
C24 C 0.1477(3) 0.1612(2) 0.5215(3) 0.0445(6) Uani 1 1 d . . . . .
H24A H 0.0347 0.1330 0.5175 0.053 Uiso 1 1 calc R . . . .
H24B H 0.2032 0.1917 0.6072 0.053 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0429(14) 2_566 ?
Ni1 O1 2.0498(14) . ?
Ni1 O2 2.0460(13) . ?
Ni1 O3 2.0588(13) . ?
Ni1 O4 2.0532(15) . ?
Ni1 O5 2.0610(15) . ?
P2 O2 1.4935(14) . ?
P2 O3 1.4955(14) 2_566 ?
P2 O6 1.6301(15) . ?
P2 O7 1.5803(13) . ?
Cl3 C13 1.724(2) . ?
Cl4 C16 1.723(2) . ?
Cl5 C12 1.722(2) . ?
Cl6 C11 1.727(2) . ?
O1 Ni1 2.0429(14) 2_566 ?
O1 C10 1.317(2) . ?
O3 P2 1.4956(14) 2_566 ?
O4 C23 1.445(3) . ?
O4 C24 1.440(3) . ?
O5 C14 1.453(2) . ?
O5 C19 1.445(3) . ?
O6 C8 1.366(2) . ?
O7 C9 1.454(2) . ?
C8 C10 1.413(3) . ?
C8 C13 1.390(3) . ?
C9 C17 1.500(3) . ?
C10 C16 1.407(3) . ?
C11 C12 1.392(3) . ?
C11 C13 1.396(3) . ?
C12 C16 1.390(3) . ?
C14 C21 1.512(3) . ?
C15 C18 1.523(3) . ?
C15 C23 1.521(3) . ?
C18 C24 1.486(4) . ?
C19 C20 1.511(4) . ?
C20 C21 1.514(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 85.28(6) 2_566 . ?
O1 Ni1 O2 87.28(6) 2_566 . ?
O1 Ni1 O3 84.39(5) 2_566 . ?
O1 Ni1 O3 86.94(5) . . ?
O1 Ni1 O4 91.37(6) 2_566 . ?
O1 Ni1 O4 176.55(6) . . ?
O1 Ni1 O5 93.72(6) . . ?
O1 Ni1 O5 178.59(6) 2_566 . ?
O2 Ni1 O1 85.17(5) . . ?
O2 Ni1 O3 168.96(6) . . ?
O2 Ni1 O4 93.85(6) . . ?
O2 Ni1 O5 93.63(6) . . ?
O3 Ni1 O5 94.57(6) . . ?
O4 Ni1 O3 93.58(6) . . ?
O4 Ni1 O5 89.64(7) . . ?
O2 P2 O3 122.13(8) . 2_566 ?
O2 P2 O6 107.95(8) . . ?
O2 P2 O7 110.20(8) . . ?
O3 P2 O6 110.09(8) 2_566 . ?
O3 P2 O7 105.81(8) 2_566 . ?
O7 P2 O6 97.97(7) . . ?
Ni1 O1 Ni1 94.72(6) 2_566 . ?
C10 O1 Ni1 131.18(12) . . ?
C10 O1 Ni1 130.24(12) . 2_566 ?
P2 O2 Ni1 117.97(8) . . ?
P2 O3 Ni1 118.35(8) 2_566 . ?
C23 O4 Ni1 122.28(13) . . ?
C24 O4 Ni1 121.17(14) . . ?
C24 O4 C23 109.06(17) . . ?
C14 O5 Ni1 120.80(13) . . ?
C19 O5 Ni1 126.00(13) . . ?
C19 O5 C14 109.83(17) . . ?
C8 O6 P2 127.47(13) . . ?
C9 O7 P2 119.62(12) . . ?
O6 C8 C10 122.25(17) . . ?
O6 C8 C13 116.53(17) . . ?
C13 C8 C10 121.22(18) . . ?
O7 C9 C17 107.73(17) . . ?
O1 C10 C8 121.53(17) . . ?
O1 C10 C16 121.76(18) . . ?
C16 C10 C8 116.71(18) . . ?
C12 C11 Cl6 120.49(16) . . ?
C12 C11 C13 119.38(19) . . ?
C13 C11 Cl6 120.11(16) . . ?
C11 C12 Cl5 119.82(16) . . ?
C16 C12 Cl5 120.38(17) . . ?
C16 C12 C11 119.80(19) . . ?
C8 C13 Cl3 119.06(16) . . ?
C8 C13 C11 120.52(19) . . ?
C11 C13 Cl3 120.40(16) . . ?
O5 C14 C21 105.46(19) . . ?
C23 C15 C18 103.85(18) . . ?
C10 C16 Cl4 117.39(16) . . ?
C12 C16 Cl4 120.37(16) . . ?
C12 C16 C10 122.24(19) . . ?
C24 C18 C15 102.65(19) . . ?
O5 C19 C20 104.7(2) . . ?
C19 C20 C21 102.1(2) . . ?
C14 C21 C20 103.0(2) . . ?
O4 C23 C15 106.09(18) . . ?
O4 C24 C18 104.58(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene and thf'
####################################################################### 
# 
# 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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2041784'
loop_
_audit_author_name
_audit_author_address
'Yile Wu'
;Ningbo University
China
;
_audit_update_record             
;
2020-11-01 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_audit_creation_date             2020-09-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H13 Cl6 O6 P Zr'
_chemical_formula_sum            'C12 H13 Cl6 O6 P Zr'
_chemical_formula_weight         588.11
_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 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.6112(5)
_cell_length_b                   11.6372(6)
_cell_length_c                   18.1370(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.301(2)
_cell_angle_gamma                90
_cell_volume                     2001.91(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.99
_cell_measurement_theta_min      4.53
_shelx_estimated_absorpt_T_max   0.698
_shelx_estimated_absorpt_T_min   0.359
_exptl_absorpt_coefficient_mu    12.894
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4941
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1419 before and 0.0906 after correction.
The Ratio of minimum to maximum transmission is 0.6557.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49347
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.443
_diffrn_reflns_theta_min         4.532
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3732
_reflns_number_total             3948
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3948
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0291
_refine_ls_restrained_S_all      1.073
_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)+(0.0463P)²+1.9516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0787
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C7(H7A,H7B), C12(H12A,H12B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_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
Zr1 Zr 0.65320(2) 0.40253(2) 0.61458(2) 0.01625(8) Uani 1 1 d . . . . .
Cl3 Cl 0.66438(7) 0.12494(5) 0.44018(3) 0.02574(14) Uani 1 1 d . . . . .
Cl1 Cl 0.57657(7) 0.30273(5) 0.71876(3) 0.02558(14) Uani 1 1 d . . . . .
Cl2 Cl 0.89095(6) 0.33106(5) 0.64128(4) 0.02737(15) Uani 1 1 d . . . . .
P1 P 0.31552(6) 0.46244(5) 0.55113(3) 0.01793(14) Uani 1 1 d . . . . .
Cl4 Cl 0.42063(8) -0.03179(5) 0.35592(4) 0.03209(16) Uani 1 1 d . . . . .
Cl6 Cl 0.04580(7) 0.20153(6) 0.49237(4) 0.03173(16) Uani 1 1 d . . . . .
Cl5 Cl 0.11201(8) 0.00598(6) 0.38296(4) 0.03788(18) Uani 1 1 d . . . . .
O5 O 0.56654(18) 0.29113(14) 0.54015(9) 0.0193(3) Uani 1 1 d . . . . .
O6 O 0.71195(18) 0.54507(14) 0.69304(9) 0.0201(3) Uani 1 1 d . . . . .
O3 O 0.29209(18) 0.48596(15) 0.46845(9) 0.0201(3) Uani 1 1 d . . . . .
O1 O 0.45848(18) 0.49457(15) 0.59346(10) 0.0206(3) Uani 1 1 d . . . . .
O2 O 0.29096(19) 0.32793(15) 0.56264(10) 0.0212(4) Uani 1 1 d . . . . .
O4 O 0.1970(2) 0.52209(17) 0.58528(11) 0.0262(4) Uani 1 1 d . . . . .
C1 C 0.3235(3) 0.2449(2) 0.51356(13) 0.0193(5) Uani 1 1 d . . . . .
C3 C 0.4921(3) 0.1422(2) 0.45356(14) 0.0211(5) Uani 1 1 d . . . . .
C2 C 0.4634(3) 0.2275(2) 0.50342(13) 0.0186(5) Uani 1 1 d . . . . .
C4 C 0.3834(3) 0.0742(2) 0.41565(14) 0.0242(5) Uani 1 1 d . . . . .
C6 C 0.2151(3) 0.1771(2) 0.47653(14) 0.0236(5) Uani 1 1 d . . . . .
C9 C 0.6678(3) 0.6655(2) 0.68046(15) 0.0236(5) Uani 1 1 d . . . . .
H9A H 0.567182 0.675034 0.685045 0.028 Uiso 1 1 calc R . . . .
H9B H 0.681791 0.691486 0.630201 0.028 Uiso 1 1 calc R . . . .
C5 C 0.2456(3) 0.0914(2) 0.42791(15) 0.0262(6) Uani 1 1 d . . . . .
C10 C 0.7611(3) 0.7324(2) 0.74068(15) 0.0247(5) Uani 1 1 d . . . . .
H10A H 0.714215 0.803712 0.753624 0.030 Uiso 1 1 calc R . . . .
H10B H 0.852211 0.752326 0.725145 0.030 Uiso 1 1 calc R . . . .
C11 C 0.7812(3) 0.6481(2) 0.80551(15) 0.0276(6) Uani 1 1 d . . . . .
H11A H 0.866764 0.666644 0.841718 0.033 Uiso 1 1 calc R . . . .
H11B H 0.698490 0.648093 0.831752 0.033 Uiso 1 1 calc R . . . .
C7 C 0.2007(3) 0.5373(3) 0.66537(16) 0.0320(6) Uani 1 1 d . . . . .
H7A H 0.298688 0.551035 0.690309 0.038 Uiso 1 1 calc R . . . .
H7B H 0.165064 0.467276 0.687113 0.038 Uiso 1 1 calc R . . . .
C12 C 0.7964(3) 0.5336(2) 0.76796(14) 0.0270(6) Uani 1 1 d . . . . .
H12A H 0.896428 0.518042 0.764525 0.032 Uiso 1 1 calc R . . . .
H12B H 0.760099 0.470365 0.796042 0.032 Uiso 1 1 calc R . . . .
C8 C 0.1103(4) 0.6377(3) 0.67684(19) 0.0406(7) Uani 1 1 d . . . . .
H8A H 0.014771 0.625178 0.649666 0.061 Uiso 1 1 calc GR . . . .
H8B H 0.149865 0.707424 0.658138 0.061 Uiso 1 1 calc GR . . . .
H8C H 0.106770 0.646414 0.730245 0.061 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
Zr1 Cl1 2.4313(6) . ?
Zr1 Cl2 2.4063(6) . ?
Zr1 O5 1.9578(17) . ?
Zr1 O6 2.1990(17) . ?
Zr1 O3 2.1176(17) 3_666 ?
Zr1 O1 2.1366(17) . ?
Cl3 C3 1.723(3) . ?
P1 O3 1.5051(18) . ?
P1 O1 1.5087(18) . ?
P1 O2 1.6016(18) . ?
P1 O4 1.5463(18) . ?
Cl4 C4 1.717(3) . ?
Cl6 C6 1.721(3) . ?
Cl5 C5 1.721(3) . ?
O5 C2 1.327(3) . ?
O6 C9 1.472(3) . ?
O6 C12 1.472(3) . ?
O2 C1 1.384(3) . ?
O4 C7 1.458(3) . ?
C1 C2 1.400(4) . ?
C1 C6 1.390(4) . ?
C3 C2 1.400(3) . ?
C3 C4 1.400(4) . ?
C4 C5 1.393(4) . ?
C6 C5 1.394(4) . ?
C9 C10 1.512(4) . ?
C10 C11 1.520(4) . ?
C11 C12 1.514(4) . ?
C7 C8 1.490(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Zr1 Cl1 94.33(2) . . ?
O5 Zr1 Cl1 94.07(5) . . ?
O5 Zr1 Cl2 101.20(5) . . ?
O5 Zr1 O6 169.05(7) . . ?
O5 Zr1 O3 92.42(7) . 3_666 ?
O5 Zr1 O1 86.88(7) . . ?
O6 Zr1 Cl1 86.32(5) . . ?
O6 Zr1 Cl2 89.68(5) . . ?
O3 Zr1 Cl1 170.62(5) 3_666 . ?
O3 Zr1 Cl2 91.04(5) 3_666 . ?
O3 Zr1 O6 86.02(6) 3_666 . ?
O3 Zr1 O1 82.90(7) 3_666 . ?
O1 Zr1 Cl1 90.70(5) . . ?
O1 Zr1 Cl2 170.13(5) . . ?
O1 Zr1 O6 82.17(7) . . ?
O3 P1 O1 116.06(10) . . ?
O3 P1 O2 107.83(10) . . ?
O3 P1 O4 108.43(10) . . ?
O1 P1 O2 108.49(10) . . ?
O1 P1 O4 110.74(10) . . ?
O4 P1 O2 104.65(10) . . ?
C2 O5 Zr1 156.28(16) . . ?
C9 O6 Zr1 125.50(14) . . ?
C9 O6 C12 109.37(18) . . ?
C12 O6 Zr1 125.07(14) . . ?
P1 O3 Zr1 143.67(11) . 3_666 ?
P1 O1 Zr1 131.78(10) . . ?
C1 O2 P1 123.05(15) . . ?
C7 O4 P1 123.55(18) . . ?
O2 C1 C2 120.5(2) . . ?
O2 C1 C6 118.5(2) . . ?
C6 C1 C2 121.0(2) . . ?
C2 C3 Cl3 117.9(2) . . ?
C4 C3 Cl3 121.5(2) . . ?
C4 C3 C2 120.6(2) . . ?
O5 C2 C1 120.6(2) . . ?
O5 C2 C3 120.7(2) . . ?
C3 C2 C1 118.7(2) . . ?
C3 C4 Cl4 120.1(2) . . ?
C5 C4 Cl4 120.3(2) . . ?
C5 C4 C3 119.6(2) . . ?
C1 C6 Cl6 118.8(2) . . ?
C1 C6 C5 119.6(2) . . ?
C5 C6 Cl6 121.6(2) . . ?
O6 C9 C10 104.8(2) . . ?
C4 C5 Cl5 119.8(2) . . ?
C4 C5 C6 120.4(2) . . ?
C6 C5 Cl5 119.8(2) . . ?
C9 C10 C11 102.3(2) . . ?
C12 C11 C10 103.3(2) . . ?
O4 C7 C8 108.3(2) . . ?
O6 C12 C11 104.9(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: thf'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2041786'
loop_
_audit_author_name
_audit_author_address
'Yile Wu'
;Ningbo University
China
;
_audit_update_record             
;
2020-11-01 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_audit_creation_date             2020-09-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.12(C24 H30 Cl10 O14 P2 V2)'
_chemical_formula_sum            'C2.82 H3.53 Cl1.18 O1.65 P0.24 V0.24'
_chemical_formula_weight         124.80
_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 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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                   12.0697(6)
_cell_length_b                   12.2097(6)
_cell_length_c                   16.6508(8)
_cell_angle_alpha                72.3790(10)
_cell_angle_beta                 73.2710(10)
_cell_angle_gamma                60.5460(10)
_cell_volume                     2007.62(17)
_cell_formula_units_Z            17
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    199(2)
_cell_measurement_theta_max      72.73
_cell_measurement_theta_min      2.82
_shelx_estimated_absorpt_T_max   0.211
_shelx_estimated_absorpt_T_min   0.164
_exptl_absorpt_coefficient_mu    11.316
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5729
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1030 before and 0.0686 after correction.
The Ratio of minimum to maximum transmission is 0.7602.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            62077
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.861
_diffrn_reflns_theta_min         2.824
_diffrn_ambient_temperature      199.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7839
_reflns_number_total             7917
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7917
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0331
_refine_ls_restrained_S_all      1.051
_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)+(0.0515P)²+1.6321P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0876
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C22(H22A,H22B), C23(H23A,H23B), C7(H7A,H7B),
 C19(H19A,H19B)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C21(H21A,H21B,
 H21C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
V1 V 0.49794(3) 0.68341(3) 0.88507(2) 0.01682(8) Uani 1 1 d . . . . .
V2 V 1.20911(3) -0.02733(3) 0.50870(2) 0.01736(8) Uani 1 1 d . . . . .
P1 P 0.30142(4) 0.59170(5) 1.02467(3) 0.01761(11) Uani 1 1 d . . . . .
Cl7 Cl 0.95491(5) 0.33822(5) 0.61697(3) 0.03014(12) Uani 1 1 d . . . . .
P2 P 1.04624(5) 0.05168(5) 0.36547(3) 0.01933(11) Uani 1 1 d . . . . .
Cl1 Cl 0.31562(5) 0.87060(5) 0.84743(3) 0.03156(12) Uani 1 1 d . . . . .
Cl2 Cl 0.15497(5) 0.41352(6) 0.97805(3) 0.03169(12) Uani 1 1 d . . . . .
Cl5 Cl 0.64744(5) 0.39343(6) 0.71832(4) 0.03366(13) Uani 1 1 d . . . . .
Cl4 Cl 0.55542(5) 0.18563(5) 0.74090(4) 0.03343(12) Uani 1 1 d . . . . .
Cl8 Cl 0.76726(5) 0.60577(5) 0.52623(4) 0.03483(13) Uani 1 1 d . . . . .
Cl3 Cl 0.30700(5) 0.19561(5) 0.87163(4) 0.03319(12) Uani 1 1 d . . . . .
Cl6 Cl 1.36649(5) 0.01534(6) 0.40643(3) 0.03434(13) Uani 1 1 d . . . . .
Cl10 Cl 0.90360(8) 0.41480(6) 0.24122(4) 0.05041(18) Uani 1 1 d . . . . .
Cl9 Cl 0.73665(8) 0.64372(6) 0.33955(5) 0.05173(19) Uani 1 1 d . . . . .
O1 O 0.40381(13) 0.63625(13) 0.99979(8) 0.0203(3) Uani 1 1 d . . . . .
O3 O 0.33557(13) 0.46061(13) 1.07944(9) 0.0209(3) Uani 1 1 d . . . . .
O9 O 1.06728(13) 0.17891(14) 0.34044(9) 0.0210(3) Uani 1 1 d . . . . .
O5 O 0.48347(14) 0.58547(14) 0.82316(9) 0.0231(3) Uani 1 1 d . . . . .
O13 O 1.29192(14) -0.04012(14) 0.60863(9) 0.0243(3) Uani 1 1 d . . . . .
O2 O 0.25807(13) 0.59658(13) 0.94054(9) 0.0214(3) Uani 1 1 d . . . . .
O12 O 1.09153(14) 0.14575(14) 0.51155(9) 0.0239(3) Uani 1 1 d . . . . .
O6 O 0.62068(14) 0.74176(14) 0.78247(9) 0.0232(3) Uani 1 1 d . . . . .
O7 O 0.53420(14) 0.79515(13) 0.93929(9) 0.0223(3) Uani 1 1 d . . . . .
O8 O 1.14051(14) -0.05023(14) 0.42143(10) 0.0264(3) Uani 1 1 d . . . . .
O4 O 0.17721(14) 0.69626(14) 1.06669(10) 0.0278(3) Uani 1 1 d . . . . .
O14 O 1.34304(15) -0.21997(14) 0.52908(11) 0.0293(3) Uani 1 1 d . . . . .
O11 O 0.90569(14) 0.09223(15) 0.39907(10) 0.0287(3) Uani 1 1 d . . . . .
O10 O 1.08708(17) 0.01076(17) 0.27749(11) 0.0359(4) Uani 1 1 d . . . . .
C2 C 0.44252(19) 0.49826(19) 0.83622(12) 0.0192(4) Uani 1 1 d . . . . .
C1 C 0.33230(18) 0.49855(19) 0.89490(12) 0.0195(4) Uani 1 1 d . . . . .
C13 C 1.01225(17) 0.25557(18) 0.47109(12) 0.0175(4) Uani 1 1 d . . . . .
C18 C 0.99671(18) 0.27641(19) 0.38661(12) 0.0191(4) Uani 1 1 d . . . . .
C14 C 0.93838(18) 0.36097(19) 0.51322(12) 0.0203(4) Uani 1 1 d . . . . .
C3 C 0.50975(19) 0.3988(2) 0.78896(12) 0.0219(4) Uani 1 1 d . . . . .
C6 C 0.29164(18) 0.4060(2) 0.90547(12) 0.0217(4) Uani 1 1 d . . . . .
C17 C 0.9151(2) 0.3953(2) 0.34615(13) 0.0265(4) Uani 1 1 d . . . . .
C15 C 0.85551(19) 0.4795(2) 0.47293(14) 0.0238(4) Uani 1 1 d . . . . .
C4 C 0.46899(19) 0.30619(19) 0.79904(13) 0.0225(4) Uani 1 1 d . . . . .
C5 C 0.35898(19) 0.30967(19) 0.85766(13) 0.0229(4) Uani 1 1 d . . . . .
C24 C 1.2947(2) 0.0684(2) 0.62381(16) 0.0321(5) Uani 1 1 d . . . . .
H24A H 1.3608 0.0880 0.5809 0.048 Uiso 1 1 calc GR . . . .
H24B H 1.3151 0.0484 0.6810 0.048 Uiso 1 1 calc GR . . . .
H24C H 1.2102 0.1427 0.6199 0.048 Uiso 1 1 calc GR . . . .
C10 C 0.5876(2) 0.8734(2) 0.87378(15) 0.0319(5) Uani 1 1 d . . . . .
H10A H 0.6285 0.9049 0.8994 0.038 Uiso 1 1 calc R . . . .
H10B H 0.5186 0.9483 0.8446 0.038 Uiso 1 1 calc R . . . .
C16 C 0.8430(2) 0.4981(2) 0.38857(15) 0.0284(4) Uani 1 1 d . . . . .
C9 C 0.4380(2) 0.8648(2) 1.00355(14) 0.0289(5) Uani 1 1 d . . . . .
H9A H 0.3662 0.9373 0.9769 0.043 Uiso 1 1 calc GR . . . .
H9B H 0.4764 0.8966 1.0301 0.043 Uiso 1 1 calc GR . . . .
H9C H 0.4060 0.8077 1.0473 0.043 Uiso 1 1 calc GR . . . .
C11 C 0.6858(2) 0.7916(2) 0.81146(14) 0.0294(5) Uani 1 1 d . . . . .
H11A H 0.7201 0.8431 0.7627 0.035 Uiso 1 1 calc R . . . .
H11B H 0.7584 0.7205 0.8394 0.035 Uiso 1 1 calc R . . . .
C12 C 0.7066(2) 0.6633(2) 0.72042(14) 0.0324(5) Uani 1 1 d . . . . .
H12A H 0.7838 0.5961 0.7441 0.049 Uiso 1 1 calc GR . . . .
H12B H 0.7317 0.7165 0.6687 0.049 Uiso 1 1 calc GR . . . .
H12C H 0.6629 0.6237 0.7061 0.049 Uiso 1 1 calc GR . . . .
C22 C 1.3895(2) -0.2615(2) 0.60879(16) 0.0348(5) Uani 1 1 d . . . . .
H22A H 1.4720 -0.3406 0.6074 0.042 Uiso 1 1 calc R . . . .
H22B H 1.3259 -0.2795 0.6566 0.042 Uiso 1 1 calc R . . . .
C23 C 1.4086(2) -0.1559(2) 0.62035(16) 0.0319(5) Uani 1 1 d . . . . .
H23A H 1.4275 -0.1742 0.6783 0.038 Uiso 1 1 calc R . . . .
H23B H 1.4820 -0.1473 0.5779 0.038 Uiso 1 1 calc R . . . .
C21 C 1.3526(3) -0.3174(2) 0.4944(2) 0.0452(6) Uani 1 1 d . . . . .
H21A H 1.3090 -0.3655 0.5369 0.068 Uiso 1 1 calc GR . . . .
H21B H 1.4437 -0.3756 0.4790 0.068 Uiso 1 1 calc GR . . . .
H21C H 1.3117 -0.2784 0.4433 0.068 Uiso 1 1 calc GR . . . .
C7 C 0.0637(2) 0.6775(3) 1.1107(2) 0.0444(6) Uani 1 1 d . . . . .
H7A H 0.0890 0.5898 1.1456 0.053 Uiso 1 1 calc R . . . .
H7B H 0.0129 0.6890 1.0690 0.053 Uiso 1 1 calc R . . . .
C19 C 0.9962(4) 0.0717(3) 0.21699(19) 0.0549(8) Uani 1 1 d . . . . .
H19A H 0.9394 0.1625 0.2218 0.066 Uiso 1 1 calc R . . . .
H19B H 0.9415 0.0272 0.2296 0.066 Uiso 1 1 calc R . . . .
C8 C -0.0142(3) 0.7744(5) 1.1666(2) 0.0707(11) Uani 1 1 d . . . . .
H8A H -0.0534 0.8597 1.1312 0.106 Uiso 1 1 calc GR . . . .
H8B H 0.0418 0.7735 1.1995 0.106 Uiso 1 1 calc GR . . . .
H8C H -0.0822 0.7537 1.2059 0.106 Uiso 1 1 calc GR . . . .
C20 C 1.0723(7) 0.0636(8) 0.1296(3) 0.135(3) Uani 1 1 d . . . . .
H20A H 1.0145 0.0916 0.0888 0.203 Uiso 1 1 calc GR . . . .
H20B H 1.1371 -0.0252 0.1278 0.203 Uiso 1 1 calc GR . . . .
H20C H 1.1154 0.1190 0.1143 0.203 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
V1 Cl1 2.3322(6) . ?
V1 O1 1.9999(13) . ?
V1 O3 2.0146(14) 2_667 ?
V1 O5 1.8917(14) . ?
V1 O6 2.1129(14) . ?
V1 O7 2.1043(14) . ?
V2 Cl6 2.3137(6) . ?
V2 O13 2.1067(14) . ?
V2 O12 1.8854(14) . ?
V2 O8 2.0104(15) . ?
V2 O14 2.0866(15) . ?
V2 O11 2.0060(15) 2_756 ?
P1 O1 1.4915(14) . ?
P1 O3 1.4991(14) . ?
P1 O2 1.6064(14) . ?
P1 O4 1.5561(14) . ?
Cl7 C14 1.719(2) . ?
P2 O9 1.6082(15) . ?
P2 O8 1.4924(15) . ?
P2 O11 1.4938(15) . ?
P2 O10 1.5567(16) . ?
Cl2 C6 1.721(2) . ?
Cl5 C3 1.722(2) . ?
Cl4 C4 1.721(2) . ?
Cl8 C15 1.723(2) . ?
Cl3 C5 1.722(2) . ?
Cl10 C17 1.728(2) . ?
Cl9 C16 1.719(2) . ?
O3 V1 2.0146(14) 2_667 ?
O9 C18 1.383(2) . ?
O5 C2 1.319(2) . ?
O13 C24 1.440(3) . ?
O13 C23 1.433(2) . ?
O2 C1 1.385(2) . ?
O12 C13 1.315(2) . ?
O6 C11 1.444(3) . ?
O6 C12 1.438(3) . ?
O7 C10 1.445(3) . ?
O7 C9 1.442(2) . ?
O4 C7 1.448(3) . ?
O14 C22 1.440(3) . ?
O14 C21 1.416(3) . ?
O11 V2 2.0060(15) 2_756 ?
O10 C19 1.467(3) . ?
C2 C1 1.405(3) . ?
C2 C3 1.412(3) . ?
C1 C6 1.387(3) . ?
C13 C18 1.402(3) . ?
C13 C14 1.415(3) . ?
C18 C17 1.384(3) . ?
C14 C15 1.386(3) . ?
C3 C4 1.391(3) . ?
C6 C5 1.390(3) . ?
C17 C16 1.392(3) . ?
C15 C16 1.394(3) . ?
C4 C5 1.393(3) . ?
C10 C11 1.495(3) . ?
C22 C23 1.491(3) . ?
C7 C8 1.489(4) . ?
C19 C20 1.483(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 Cl1 92.96(4) . . ?
O1 V1 O3 89.09(6) . 2_667 ?
O1 V1 O6 165.51(6) . . ?
O1 V1 O7 88.19(6) . . ?
O3 V1 Cl1 171.30(5) 2_667 . ?
O3 V1 O6 84.09(6) 2_667 . ?
O3 V1 O7 85.35(6) 2_667 . ?
O5 V1 Cl1 95.29(5) . . ?
O5 V1 O1 99.66(6) . . ?
O5 V1 O3 92.69(6) . 2_667 ?
O5 V1 O6 93.44(6) . . ?
O5 V1 O7 171.88(6) . . ?
O6 V1 Cl1 91.97(4) . . ?
O7 V1 Cl1 86.26(4) . . ?
O7 V1 O6 78.54(6) . . ?
O13 V2 Cl6 91.69(4) . . ?
O12 V2 Cl6 95.60(5) . . ?
O12 V2 O13 91.82(6) . . ?
O12 V2 O8 97.60(6) . . ?
O12 V2 O14 168.92(6) . . ?
O12 V2 O11 92.99(7) . 2_756 ?
O8 V2 Cl6 92.35(5) . . ?
O8 V2 O13 169.34(6) . . ?
O8 V2 O14 92.59(6) . . ?
O14 V2 Cl6 88.29(5) . . ?
O14 V2 O13 77.67(6) . . ?
O11 V2 Cl6 171.10(5) 2_756 . ?
O11 V2 O13 85.69(6) 2_756 . ?
O11 V2 O8 88.83(7) 2_756 . ?
O11 V2 O14 82.84(7) 2_756 . ?
O1 P1 O3 115.86(8) . . ?
O1 P1 O2 109.80(8) . . ?
O1 P1 O4 107.31(8) . . ?
O3 P1 O2 108.72(8) . . ?
O3 P1 O4 112.21(8) . . ?
O4 P1 O2 102.04(8) . . ?
O8 P2 O9 109.27(8) . . ?
O8 P2 O11 118.18(9) . . ?
O8 P2 O10 107.55(9) . . ?
O11 P2 O9 106.54(8) . . ?
O11 P2 O10 112.12(10) . . ?
O10 P2 O9 101.95(9) . . ?
P1 O1 V1 131.10(9) . . ?
P1 O3 V1 133.26(8) . 2_667 ?
C18 O9 P2 122.05(12) . . ?
C2 O5 V1 139.82(13) . . ?
C24 O13 V2 122.74(12) . . ?
C23 O13 V2 112.59(13) . . ?
C23 O13 C24 113.04(16) . . ?
C1 O2 P1 119.82(12) . . ?
C13 O12 V2 147.01(13) . . ?
C11 O6 V1 111.12(12) . . ?
C12 O6 V1 121.93(13) . . ?
C12 O6 C11 111.07(16) . . ?
C10 O7 V1 110.80(12) . . ?
C9 O7 V1 120.24(13) . . ?
C9 O7 C10 112.19(16) . . ?
P2 O8 V2 127.53(9) . . ?
C7 O4 P1 122.96(15) . . ?
C22 O14 V2 112.97(13) . . ?
C21 O14 V2 126.10(15) . . ?
C21 O14 C22 116.01(18) . . ?
P2 O11 V2 139.07(9) . 2_756 ?
C19 O10 P2 120.38(18) . . ?
O5 C2 C1 123.57(18) . . ?
O5 C2 C3 119.85(17) . . ?
C1 C2 C3 116.57(18) . . ?
O2 C1 C2 119.77(17) . . ?
O2 C1 C6 118.60(17) . . ?
C6 C1 C2 121.55(18) . . ?
O12 C13 C18 123.80(18) . . ?
O12 C13 C14 119.44(17) . . ?
C18 C13 C14 116.75(17) . . ?
O9 C18 C13 120.32(17) . . ?
O9 C18 C17 118.28(17) . . ?
C17 C18 C13 121.35(18) . . ?
C13 C14 Cl7 117.83(15) . . ?
C15 C14 Cl7 120.38(16) . . ?
C15 C14 C13 121.78(18) . . ?
C2 C3 Cl5 117.76(15) . . ?
C4 C3 Cl5 120.16(16) . . ?
C4 C3 C2 122.08(18) . . ?
C1 C6 Cl2 118.80(16) . . ?
C1 C6 C5 120.74(18) . . ?
C5 C6 Cl2 120.46(16) . . ?
C18 C17 Cl10 118.76(17) . . ?
C18 C17 C16 121.16(19) . . ?
C16 C17 Cl10 120.08(16) . . ?
C14 C15 Cl8 120.48(16) . . ?
C14 C15 C16 120.31(19) . . ?
C16 C15 Cl8 119.22(16) . . ?
C3 C4 Cl4 120.33(16) . . ?
C3 C4 C5 119.80(19) . . ?
C5 C4 Cl4 119.86(16) . . ?
C6 C5 Cl3 120.08(16) . . ?
C6 C5 C4 119.26(19) . . ?
C4 C5 Cl3 120.66(16) . . ?
O7 C10 C11 107.39(17) . . ?
C17 C16 Cl9 120.99(17) . . ?
C17 C16 C15 118.64(19) . . ?
C15 C16 Cl9 120.34(17) . . ?
O6 C11 C10 106.61(18) . . ?
O14 C22 C23 107.25(18) . . ?
O13 C23 C22 107.51(17) . . ?
O4 C7 C8 107.3(2) . . ?
O10 C19 C20 107.9(3) . . ?

_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_1_a
_database_code_depnum_ccdc_archive 'CCDC 2023193'
loop_
_audit_author_name
_audit_author_address
'Yile Wu'
;Ningbo University
China
;
_audit_update_record             
;
2020-08-13 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_audit_creation_date             2020-08-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C16 H21 Cl5 O7 P V), 2(C4 H8 O)'
_chemical_formula_sum            'C40 H58 Cl10 O16 P2 V2'
_chemical_formula_weight         1313.18
_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 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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                   14.4834(9)
_cell_length_b                   14.9881(9)
_cell_length_c                   15.5710(10)
_cell_angle_alpha                107.350(2)
_cell_angle_beta                 117.247(2)
_cell_angle_gamma                98.551(2)
_cell_volume                     2701.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.16
_cell_measurement_theta_min      3.51
_shelx_estimated_absorpt_T_max   0.019
_shelx_estimated_absorpt_T_min   0.014
_exptl_absorpt_coefficient_mu    8.563
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1411 before and 0.0836 after correction.
The Ratio of minimum to maximum transmission is 0.5143.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            82763
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.297
_diffrn_reflns_theta_min         3.512
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10114
_reflns_number_total             10538
_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 V8.40A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         10538
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.044
_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)+(0.0718P)²+3.9221P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1174
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C29(H29A,H29B), C28(H28A,H28B), C23(H23A,H23B), C7(H7A,H7B),
 C32(H32A,H32B), C27(H27A,H27B), C25(H25A,H25B), C10(H10A,H10B), C37(H37A,H37B),
  C11(H11A,H11B), C26(H26A,H26B), C30(H30A,H30B), C31(H31A,H31B), C40(H40A,
 H40B), C9(H9A,H9B), C38(H38A,H38B), C39(H39A,H39B), C34(H34A,H34B), C35(H35A,
 H35B), C33(H33A,H33B), C36(H36A,H36B), C01V(H01A,H01B), C01W(H01C,H01D),
 C01X(H01E,H01F), C01Y(H01G,H01H)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
V1 V 0.12179(3) 0.53329(3) 0.42191(3) 0.00801(10) Uani 1 1 d . . . . .
V2 V 0.61559(3) 0.55052(3) 0.92404(3) 0.00801(10) Uani 1 1 d . . . . .
Cl2 Cl 0.56153(5) 0.50880(4) 0.74634(4) 0.01471(12) Uani 1 1 d . . . . .
P1 P -0.12498(4) 0.40767(4) 0.35580(4) 0.00752(12) Uani 1 1 d . . . . .
Cl3 Cl -0.23323(5) 0.12474(4) 0.19673(5) 0.01645(13) Uani 1 1 d . . . . .
Cl4 Cl -0.14506(5) 0.01478(4) 0.06079(5) 0.01888(13) Uani 1 1 d . . . . .
Cl1 Cl 0.06678(4) 0.49106(4) 0.24364(4) 0.01459(12) Uani 1 1 d . . . . .
Cl6 Cl 0.24185(4) 0.32084(4) 0.31268(4) 0.01619(13) Uani 1 1 d . . . . .
Cl10 Cl 0.77399(5) 0.37550(4) 0.83658(4) 0.01695(13) Uani 1 1 d . . . . .
P2 P 0.37732(4) 0.40016(4) 0.85236(4) 0.00839(12) Uani 1 1 d . . . . .
Cl5 Cl 0.09412(5) 0.11198(4) 0.12064(5) 0.02035(14) Uani 1 1 d . . . . .
Cl7 Cl 0.30494(5) 0.11902(4) 0.68515(5) 0.02051(14) Uani 1 1 d . . . . .
Cl9 Cl 0.66130(5) 0.16522(5) 0.64770(5) 0.02282(14) Uani 1 1 d . . . . .
Cl8 Cl 0.42384(6) 0.03731(5) 0.56784(5) 0.02534(15) Uani 1 1 d . . . . .
O12 O 0.45770(13) 0.49480(11) 0.87951(12) 0.0101(3) Uani 1 1 d . . . . .
O1 O -0.17490(13) 0.41994(12) 0.42194(12) 0.0098(3) Uani 1 1 d . . . . .
O4 O -0.03593(13) 0.49574(11) 0.38300(12) 0.0096(3) Uani 1 1 d . . . . .
O5 O 0.13155(13) 0.40659(12) 0.41572(12) 0.0103(3) Uani 1 1 d . . . . .
O3 O -0.07844(13) 0.31804(12) 0.36773(12) 0.0104(3) Uani 1 1 d . . . . .
O11 O 0.64168(13) 0.43015(12) 0.92410(12) 0.0111(3) Uani 1 1 d . . . . .
O8 O 0.33086(13) 0.40262(12) 0.92046(12) 0.0109(3) Uani 1 1 d . . . . .
O10 O 0.43414(14) 0.31578(12) 0.86082(13) 0.0119(3) Uani 1 1 d . . . . .
O6 O 0.28547(13) 0.58861(13) 0.47414(12) 0.0133(3) Uani 1 1 d . . . . .
O14 O 0.59560(13) 0.68613(12) 0.93696(13) 0.0127(3) Uani 1 1 d . . . . .
O9 O 0.27746(14) 0.35705(12) 0.73497(13) 0.0146(3) Uani 1 1 d . . . . .
O2 O -0.22097(14) 0.36571(12) 0.23659(12) 0.0126(3) Uani 1 1 d . . . . .
O7 O 0.11934(14) 0.67397(12) 0.43769(13) 0.0144(3) Uani 1 1 d . . . . .
O13 O 0.77693(13) 0.61965(13) 0.97780(13) 0.0128(3) Uani 1 1 d . . . . .
C1 C -0.03916(19) 0.27244(16) 0.30697(17) 0.0098(4) Uani 1 1 d . . . . .
C3 C -0.0630(2) 0.12951(16) 0.16567(17) 0.0127(4) Uani 1 1 d . . . . .
C6 C 0.06861(19) 0.31923(17) 0.33518(17) 0.0102(4) Uani 1 1 d . . . . .
C17 C 0.4846(2) 0.28343(17) 0.80664(18) 0.0113(4) Uani 1 1 d . . . . .
C22 C 0.5908(2) 0.34235(17) 0.84246(18) 0.0115(4) Uani 1 1 d . . . . .
C18 C 0.4339(2) 0.18940(18) 0.72340(19) 0.0147(5) Uani 1 1 d . . . . .
C2 C -0.10310(18) 0.17878(17) 0.22444(18) 0.0113(4) Uani 1 1 d . . . . .
C5 C 0.10879(19) 0.26692(17) 0.27671(18) 0.0119(4) Uani 1 1 d . . . . .
C4 C 0.0432(2) 0.17382(17) 0.19225(18) 0.0134(5) Uani 1 1 d . . . . .
O15 O 0.5114(2) 0.86760(18) 0.7523(2) 0.0467(6) Uani 1 1 d . . . . .
O16 O -0.0050(3) 0.87761(19) 0.2614(2) 0.0525(7) Uani 1 1 d . . . . .
C21 C 0.64374(19) 0.30381(18) 0.79165(18) 0.0128(4) Uani 1 1 d . . . . .
C19 C 0.4869(2) 0.15304(18) 0.67225(18) 0.0162(5) Uani 1 1 d . . . . .
C20 C 0.5922(2) 0.21022(18) 0.70727(19) 0.0160(5) Uani 1 1 d . . . . .
C12 C 0.3288(2) 0.6144(2) 0.4132(2) 0.0202(5) Uani 1 1 d . . . . .
H12A H 0.2883 0.6521 0.3760 0.024 Uiso 1 1 calc R . . . .
H12B H 0.3234 0.5540 0.3601 0.024 Uiso 1 1 calc R . . . .
C29 C 0.6727(2) 0.78182(17) 1.02619(19) 0.0155(5) Uani 1 1 d . . . . .
H29A H 0.7332 0.8082 1.0176 0.019 Uiso 1 1 calc R . . . .
H29B H 0.7048 0.7747 1.0942 0.019 Uiso 1 1 calc R . . . .
C28 C 0.8176(2) 0.6508(2) 0.9169(2) 0.0182(5) Uani 1 1 d . . . . .
H28A H 0.7808 0.6952 0.8892 0.022 Uiso 1 1 calc R . . . .
H28B H 0.8048 0.5926 0.8567 0.022 Uiso 1 1 calc R . . . .
C8 C -0.2074(2) 0.31899(19) 0.07963(19) 0.0182(5) Uani 1 1 d . . . . .
H8A H -0.2152 0.3377 0.0221 0.027 Uiso 1 1 calc GR . . . .
H8B H -0.2649 0.2556 0.0500 0.027 Uiso 1 1 calc GR . . . .
H8C H -0.1347 0.3122 0.1164 0.027 Uiso 1 1 calc GR . . . .
C23 C 0.2732(2) 0.38903(18) 0.65348(18) 0.0152(5) Uani 1 1 d . . . . .
H23A H 0.3323 0.4535 0.6875 0.018 Uiso 1 1 calc R . . . .
H23B H 0.2014 0.3981 0.6147 0.018 Uiso 1 1 calc R . . . .
C7 C -0.2186(2) 0.39827(18) 0.15739(18) 0.0139(5) Uani 1 1 d . . . . .
H7A H -0.1557 0.4604 0.1935 0.017 Uiso 1 1 calc R . . . .
H7B H -0.2874 0.4118 0.1187 0.017 Uiso 1 1 calc R . . . .
C32 C 0.4944(2) 0.70097(18) 0.8691(2) 0.0168(5) Uani 1 1 d . . . . .
H32A H 0.4301 0.6393 0.8300 0.020 Uiso 1 1 calc R . . . .
H32B H 0.5006 0.7232 0.8176 0.020 Uiso 1 1 calc R . . . .
C27 C 0.9397(2) 0.7052(2) 0.9965(2) 0.0242(6) Uani 1 1 d . . . . .
H27A H 0.9544 0.7750 1.0402 0.029 Uiso 1 1 calc R . . . .
H27B H 0.9815 0.7037 0.9608 0.029 Uiso 1 1 calc R . . . .
C25 C 0.8691(2) 0.6214(2) 1.0730(2) 0.0199(5) Uani 1 1 d . . . . .
H25A H 0.8548 0.5562 1.0763 0.024 Uiso 1 1 calc R . . . .
H25B H 0.8810 0.6728 1.1378 0.024 Uiso 1 1 calc R . . . .
C10 C 0.4799(2) 0.6297(2) 0.5742(2) 0.0250(6) Uani 1 1 d . . . . .
H10A H 0.5089 0.5766 0.5540 0.030 Uiso 1 1 calc R . . . .
H10B H 0.5368 0.6796 0.6471 0.030 Uiso 1 1 calc R . . . .
C37 C 0.2036(2) 0.76740(18) 0.52584(19) 0.0187(5) Uani 1 1 d . . . . .
H37A H 0.2668 0.7849 0.5175 0.022 Uiso 1 1 calc R . . . .
H37B H 0.2307 0.7622 0.5946 0.022 Uiso 1 1 calc R . . . .
C11 C 0.4478(2) 0.6775(2) 0.4959(2) 0.0253(6) Uani 1 1 d . . . . .
H11A H 0.4549 0.7475 0.5305 0.030 Uiso 1 1 calc R . . . .
H11B H 0.4937 0.6749 0.4643 0.030 Uiso 1 1 calc R . . . .
C26 C 0.9683(2) 0.6451(2) 1.0635(2) 0.0248(6) Uani 1 1 d . . . . .
H26A H 0.9777 0.5837 1.0273 0.030 Uiso 1 1 calc R . . . .
H26B H 1.0365 0.6847 1.1341 0.030 Uiso 1 1 calc R . . . .
C30 C 0.6045(2) 0.85076(19) 1.0241(2) 0.0217(5) Uani 1 1 d . . . . .
H30A H 0.6218 0.8994 0.9978 0.026 Uiso 1 1 calc R . . . .
H30B H 0.6186 0.8870 1.0958 0.026 Uiso 1 1 calc R . . . .
C31 C 0.4850(2) 0.78086(19) 0.9477(2) 0.0216(5) Uani 1 1 d . . . . .
H31A H 0.4568 0.7534 0.9849 0.026 Uiso 1 1 calc R . . . .
H31B H 0.4362 0.8149 0.9125 0.026 Uiso 1 1 calc R . . . .
C24 C 0.2875(2) 0.3127(2) 0.5767(2) 0.0235(6) Uani 1 1 d . . . . .
H24A H 0.2757 0.3307 0.5178 0.035 Uiso 1 1 calc GR . . . .
H24B H 0.2339 0.2475 0.5490 0.035 Uiso 1 1 calc GR . . . .
H24C H 0.3624 0.3102 0.6134 0.035 Uiso 1 1 calc GR . . . .
C40 C 0.0243(2) 0.69616(19) 0.3694(2) 0.0202(5) Uani 1 1 d . . . . .
H40A H -0.0448 0.6395 0.3319 0.024 Uiso 1 1 calc R . . . .
H40B H 0.0338 0.7128 0.3163 0.024 Uiso 1 1 calc R . . . .
C9 C 0.3747(2) 0.5875(3) 0.5677(2) 0.0344(8) Uani 1 1 d . . . . .
H9A H 0.3647 0.5188 0.5621 0.041 Uiso 1 1 calc R . . . .
H9B H 0.3766 0.6282 0.6320 0.041 Uiso 1 1 calc R . . . .
C38 C 0.1462(3) 0.8452(2) 0.5206(2) 0.0333(7) Uani 1 1 d . . . . .
H38A H 0.1630 0.8874 0.5919 0.040 Uiso 1 1 calc R . . . .
H38B H 0.1694 0.8880 0.4914 0.040 Uiso 1 1 calc R . . . .
C39 C 0.0238(3) 0.7841(2) 0.4465(2) 0.0290(6) Uani 1 1 d . . . . .
H39A H -0.0072 0.7639 0.4855 0.035 Uiso 1 1 calc R . . . .
H39B H -0.0188 0.8212 0.4102 0.035 Uiso 1 1 calc R . . . .
C34 C 0.6533(3) 1.0098(3) 0.8077(3) 0.0371(7) Uani 1 1 d . . . . .
H34A H 0.6307 1.0247 0.7447 0.045 Uiso 1 1 calc R . . . .
H34B H 0.7338 1.0431 0.8583 0.045 Uiso 1 1 calc R . . . .
C35 C 0.5899(3) 1.0407(3) 0.8596(3) 0.0373(7) Uani 1 1 d . . . . .
H35A H 0.5742 1.1015 0.8542 0.045 Uiso 1 1 calc R . . . .
H35B H 0.6305 1.0519 0.9352 0.045 Uiso 1 1 calc R . . . .
C33 C 0.6211(3) 0.8996(3) 0.7767(3) 0.0377(7) Uani 1 1 d . . . . .
H33A H 0.6252 0.8653 0.7141 0.045 Uiso 1 1 calc R . . . .
H33B H 0.6711 0.8850 0.8361 0.045 Uiso 1 1 calc R . . . .
C36 C 0.4848(3) 0.9513(3) 0.7940(3) 0.0406(8) Uani 1 1 d . . . . .
H36A H 0.4572 0.9409 0.8391 0.049 Uiso 1 1 calc R . . . .
H36B H 0.4269 0.9616 0.7355 0.049 Uiso 1 1 calc R . . . .
C01V C -0.0518(3) 0.9466(4) 0.2968(4) 0.0530(11) Uani 1 1 d . . . . .
H01A H -0.0927 0.9201 0.3253 0.064 Uiso 1 1 calc R . . . .
H01B H -0.1026 0.9612 0.2380 0.064 Uiso 1 1 calc R . . . .
C01W C 0.0836(4) 0.9357(3) 0.2640(3) 0.0493(9) Uani 1 1 d . . . . .
H01C H 0.0563 0.9471 0.1986 0.059 Uiso 1 1 calc R . . . .
H01D H 0.1384 0.9017 0.2697 0.059 Uiso 1 1 calc R . . . .
C01X C 0.1343(3) 1.0318(3) 0.3591(3) 0.0480(10) Uani 1 1 d . . . . .
H01E H 0.2007 1.0318 0.4195 0.058 Uiso 1 1 calc R . . . .
H01F H 0.1557 1.0879 0.3432 0.058 Uiso 1 1 calc R . . . .
C01Y C 0.0477(4) 1.0400(3) 0.3845(3) 0.0584(12) Uani 1 1 d . . . . .
H01G H 0.0297 1.1008 0.3827 0.070 Uiso 1 1 calc R . . . .
H01H H 0.0718 1.0410 0.4556 0.070 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 Cl1 2.3491(6) . ?
V1 O1 2.0263(16) 2_566 ?
V1 O4 2.0123(16) . ?
V1 O5 1.9022(16) . ?
V1 O6 2.0534(17) . ?
V1 O7 2.0564(17) . ?
V2 Cl2 2.3450(6) . ?
V2 O12 2.0106(16) . ?
V2 O11 1.8976(16) . ?
V2 O8 2.0153(16) 2_667 ?
V2 O14 2.0592(16) . ?
V2 O13 2.0509(17) . ?
P1 O1 1.4917(16) . ?
P1 O4 1.4985(16) . ?
P1 O3 1.6116(16) . ?
P1 O2 1.5667(16) . ?
Cl3 C2 1.728(2) . ?
Cl4 C3 1.725(2) . ?
Cl6 C5 1.720(2) . ?
Cl10 C21 1.716(2) . ?
P2 O12 1.4990(16) . ?
P2 O8 1.4885(16) . ?
P2 O10 1.6136(16) . ?
P2 O9 1.5644(17) . ?
Cl5 C4 1.727(2) . ?
Cl7 C18 1.726(3) . ?
Cl9 C20 1.731(2) . ?
Cl8 C19 1.724(2) . ?
O1 V1 2.0262(16) 2_566 ?
O5 C6 1.318(3) . ?
O3 C1 1.382(3) . ?
O11 C22 1.322(3) . ?
O8 V2 2.0154(16) 2_667 ?
O10 C17 1.380(3) . ?
O6 C12 1.462(3) . ?
O6 C9 1.445(3) . ?
O14 C29 1.466(3) . ?
O14 C32 1.460(3) . ?
O9 C23 1.464(3) . ?
O2 C7 1.467(3) . ?
O7 C37 1.465(3) . ?
O7 C40 1.464(3) . ?
O13 C28 1.469(3) . ?
O13 C25 1.461(3) . ?
C1 C6 1.408(3) . ?
C1 C2 1.388(3) . ?
C3 C2 1.390(3) . ?
C3 C4 1.389(3) . ?
C6 C5 1.406(3) . ?
C17 C22 1.405(3) . ?
C17 C18 1.392(3) . ?
C22 C21 1.401(3) . ?
C18 C19 1.395(4) . ?
C5 C4 1.395(3) . ?
O15 C33 1.419(4) . ?
O15 C36 1.425(4) . ?
O16 C01V 1.429(5) . ?
O16 C01W 1.415(5) . ?
C21 C20 1.394(3) . ?
C19 C20 1.388(4) . ?
C12 C11 1.510(4) . ?
C29 C30 1.529(3) . ?
C28 C27 1.513(4) . ?
C8 C7 1.511(3) . ?
C23 C24 1.505(4) . ?
C32 C31 1.509(4) . ?
C27 C26 1.531(4) . ?
C25 C26 1.512(4) . ?
C10 C11 1.523(4) . ?
C10 C9 1.506(4) . ?
C37 C38 1.529(4) . ?
C30 C31 1.530(4) . ?
C40 C39 1.499(4) . ?
C38 C39 1.526(5) . ?
C34 C35 1.514(5) . ?
C34 C33 1.506(5) . ?
C35 C36 1.520(5) . ?
C01V C01Y 1.535(7) . ?
C01W C01X 1.491(5) . ?
C01X C01Y 1.489(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 Cl1 175.79(5) 2_566 . ?
O1 V1 O6 85.26(6) 2_566 . ?
O1 V1 O7 87.47(7) 2_566 . ?
O4 V1 Cl1 91.55(5) . . ?
O4 V1 O1 90.44(6) . 2_566 ?
O4 V1 O6 172.88(7) . . ?
O4 V1 O7 88.22(7) . . ?
O5 V1 Cl1 93.86(5) . . ?
O5 V1 O1 89.72(7) . 2_566 ?
O5 V1 O4 93.75(7) . . ?
O5 V1 O6 91.90(7) . . ?
O5 V1 O7 176.58(7) . . ?
O6 V1 Cl1 92.38(5) . . ?
O6 V1 O7 85.93(7) . . ?
O7 V1 Cl1 88.88(5) . . ?
O12 V2 Cl2 90.52(5) . . ?
O12 V2 O8 92.47(7) . 2_667 ?
O12 V2 O14 89.04(7) . . ?
O12 V2 O13 174.71(7) . . ?
O11 V2 Cl2 94.57(5) . . ?
O11 V2 O12 92.65(7) . . ?
O11 V2 O8 88.80(7) . 2_667 ?
O11 V2 O14 175.43(7) . . ?
O11 V2 O13 91.66(7) . . ?
O8 V2 Cl2 175.39(5) 2_667 . ?
O8 V2 O14 86.88(7) 2_667 . ?
O8 V2 O13 84.55(7) 2_667 . ?
O14 V2 Cl2 89.66(5) . . ?
O13 V2 Cl2 92.20(5) . . ?
O13 V2 O14 86.44(7) . . ?
O1 P1 O4 117.83(9) . . ?
O1 P1 O3 103.47(9) . . ?
O1 P1 O2 107.83(9) . . ?
O4 P1 O3 110.45(9) . . ?
O4 P1 O2 110.97(9) . . ?
O2 P1 O3 105.38(9) . . ?
O12 P2 O10 110.84(9) . . ?
O12 P2 O9 111.18(9) . . ?
O8 P2 O12 117.65(9) . . ?
O8 P2 O10 103.29(9) . . ?
O8 P2 O9 107.04(9) . . ?
O9 P2 O10 105.98(9) . . ?
P2 O12 V2 139.81(10) . . ?
P1 O1 V1 137.39(10) . 2_566 ?
P1 O4 V1 139.10(10) . . ?
C6 O5 V1 127.95(14) . . ?
C1 O3 P1 122.94(14) . . ?
C22 O11 V2 126.94(14) . . ?
P2 O8 V2 138.83(10) . 2_667 ?
C17 O10 P2 124.90(14) . . ?
C12 O6 V1 125.91(14) . . ?
C9 O6 V1 124.06(15) . . ?
C9 O6 C12 108.78(19) . . ?
C29 O14 V2 125.41(13) . . ?
C32 O14 V2 125.31(14) . . ?
C32 O14 C29 108.44(17) . . ?
C23 O9 P2 125.24(15) . . ?
C7 O2 P1 125.10(14) . . ?
C37 O7 V1 126.47(14) . . ?
C40 O7 V1 124.48(14) . . ?
C40 O7 C37 108.50(18) . . ?
C28 O13 V2 126.20(14) . . ?
C25 O13 V2 122.50(14) . . ?
C25 O13 C28 109.63(18) . . ?
O3 C1 C6 118.9(2) . . ?
O3 C1 C2 119.6(2) . . ?
C2 C1 C6 121.3(2) . . ?
C2 C3 Cl4 120.03(18) . . ?
C4 C3 Cl4 120.72(18) . . ?
C4 C3 C2 119.2(2) . . ?
O5 C6 C1 121.9(2) . . ?
O5 C6 C5 120.8(2) . . ?
C5 C6 C1 117.2(2) . . ?
O10 C17 C22 119.3(2) . . ?
O10 C17 C18 119.6(2) . . ?
C18 C17 C22 120.8(2) . . ?
O11 C22 C17 121.5(2) . . ?
O11 C22 C21 120.4(2) . . ?
C21 C22 C17 118.1(2) . . ?
C17 C18 Cl7 118.75(19) . . ?
C17 C18 C19 120.4(2) . . ?
C19 C18 Cl7 120.87(19) . . ?
C1 C2 Cl3 118.62(18) . . ?
C1 C2 C3 120.6(2) . . ?
C3 C2 Cl3 120.79(18) . . ?
C6 C5 Cl6 118.04(18) . . ?
C4 C5 Cl6 120.72(18) . . ?
C4 C5 C6 121.2(2) . . ?
C3 C4 Cl5 119.38(18) . . ?
C3 C4 C5 120.4(2) . . ?
C5 C4 Cl5 120.25(19) . . ?
C33 O15 C36 109.5(3) . . ?
C01W O16 C01V 105.0(3) . . ?
C22 C21 Cl10 117.88(18) . . ?
C20 C21 Cl10 121.10(19) . . ?
C20 C21 C22 121.0(2) . . ?
C18 C19 Cl8 120.6(2) . . ?
C20 C19 Cl8 119.97(19) . . ?
C20 C19 C18 119.4(2) . . ?
C21 C20 Cl9 119.4(2) . . ?
C19 C20 Cl9 120.29(19) . . ?
C19 C20 C21 120.3(2) . . ?
O6 C12 C11 104.03(19) . . ?
O14 C29 C30 105.65(19) . . ?
O13 C28 C27 104.22(19) . . ?
O9 C23 C24 110.0(2) . . ?
O2 C7 C8 110.13(19) . . ?
O14 C32 C31 102.85(19) . . ?
C28 C27 C26 101.8(2) . . ?
O13 C25 C26 105.5(2) . . ?
C9 C10 C11 104.7(2) . . ?
O7 C37 C38 105.3(2) . . ?
C12 C11 C10 102.8(2) . . ?
C25 C26 C27 103.0(2) . . ?
C29 C30 C31 104.1(2) . . ?
C32 C31 C30 102.1(2) . . ?
O7 C40 C39 103.0(2) . . ?
O6 C9 C10 107.1(2) . . ?
C39 C38 C37 104.1(2) . . ?
C40 C39 C38 102.1(2) . . ?
C33 C34 C35 102.3(3) . . ?
C34 C35 C36 101.9(3) . . ?
O15 C33 C34 106.4(3) . . ?
O15 C36 C35 107.1(3) . . ?
O16 C01V C01Y 104.6(3) . . ?
O16 C01W C01X 106.6(3) . . ?
C01Y C01X C01W 105.3(3) . . ?
C01X C01Y C01V 104.0(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
