Oxyphosphoranes as precursors to bridging phosphate-catecholate ligands.
Yang, Xin; Wei, Rui; Shi, Yaping; Liu, Liu Leo; Wu, Yile; Zhao, Yufen; Stephan, Douglas W.; Chemical communications (Cambridge, England) 57 (2021) 1194–1197; doi:10.1039/d0cc07736d

data_7127774
_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         '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
_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
_audit_creation_date             2020-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-01 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                72.3790(10)
_cell_angle_beta                 73.2710(10)
_cell_angle_gamma                60.5460(10)
_cell_formula_units_Z            17
_cell_length_a                   12.0697(6)
_cell_length_b                   12.2097(6)
_cell_length_c                   16.6508(8)
_cell_measurement_reflns_used    9588
_cell_measurement_temperature    199(2)
_cell_measurement_theta_max      72.73
_cell_measurement_theta_min      2.82
_cell_volume                     2007.62(17)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      199.0
_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       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_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_standards_number         0
_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 \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.755
_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
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.089
_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_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0331
_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/[\s^2^(Fo^2^)+(0.0515P)^2^+1.6321P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7839
_reflns_number_total             7917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07736d2.cif
_cod_data_source_block           1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7127772--7127775.cif.'
_cod_database_code               7127774
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.211
_shelx_estimated_absorpt_t_min   0.164
_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)
;
_shelx_res_checksum              53195
_olex2_submission_special_instructions 'No special instructions were received'