#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/77/7127772.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7127772
loop_
_publ_author_name
'Yang, Xin'
'Wei, Rui'
'Shi, Yaping'
'Liu, Liu Leo'
'Wu, Yile'
'Zhao, Yufen'
'Stephan, Douglas W.'
_publ_section_title
;
 Oxyphosphoranes as precursors to bridging phosphate-catecholate ligands.
;
_journal_issue                   10
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1194
_journal_page_last               1197
_journal_paper_doi               10.1039/d0cc07736d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C32 H42 Cl8 Ni2 O14 P2'
_chemical_formula_sum            'C32 H42 Cl8 Ni2 O14 P2'
_chemical_formula_weight         1113.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-13 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                108.4832(15)
_cell_angle_beta                 97.6582(16)
_cell_angle_gamma                100.3215(15)
_cell_formula_units_Z            1
_cell_length_a                   8.9110(5)
_cell_length_b                   11.1675(6)
_cell_length_c                   11.8597(7)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      73.47
_cell_measurement_theta_min      4.30
_cell_volume                     1078.12(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_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)'
_diffrn_ambient_temperature      103.0
_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_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_standards_number         0
_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_description       block
_exptl_crystal_F_000             568
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene and thf'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.088
_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_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0325
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4183
_reflns_number_total             4260
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc07736d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7127772--7127775.cif.'
_cod_database_code               7127772
_shelxl_version_number           2013-2
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.387
_shelx_estimated_absorpt_t_min   0.370
_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)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 . . . .
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'
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) . . ?
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_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168352485
