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_7127775
_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         '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
_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             2020-08-13
_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                107.350(2)
_cell_angle_beta                 117.247(2)
_cell_angle_gamma                98.551(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4834(9)
_cell_length_b                   14.9881(9)
_cell_length_c                   15.5710(10)
_cell_measurement_reflns_used    9334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.16
_cell_measurement_theta_min      3.51
_cell_volume                     2701.5(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_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)'
_diffrn_ambient_temperature      100.0
_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       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_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_standards_number         0
_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 \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.614
_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
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.103
_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_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0718P)^2^+3.9221P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10114
_reflns_number_total             10538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07736d2.cif
_cod_data_source_block           1_a
_cod_depositor_comments
'Adding full bibliography for 7127772--7127775.cif.'
_cod_database_code               7127775
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.019
_shelx_estimated_absorpt_t_min   0.014
_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)
;
_shelx_res_checksum              4912
_olex2_submission_special_instructions 'No special instructions were received'