The chemistry of phosphirane-substituted phosphinidene complexes.
Wang, Min; Yang, Tingting; Tian, Rongqiang; Wei, Donghui; Duan, Zheng; Mathey, François; Chemical communications (Cambridge, England) 56 (2020) 9707–9710; doi:10.1039/d0cc04501b

data_7126922
_publ_section_title
;
 The chemistry of phosphirane-substituted phosphinidene complexes.
;
_journal_issue                   67
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9707
_journal_page_last               9710
_journal_paper_doi               10.1039/d0cc04501b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C22 H20 O10 P2 W2'
_chemical_formula_sum            'C22 H20 O10 P2 W2'
_chemical_formula_weight         874.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-20 deposited with the CCDC.	2020-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.165(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8615(2)
_cell_length_b                   14.1665(2)
_cell_length_c                   17.7114(3)
_cell_measurement_reflns_used    12848
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.9610
_cell_measurement_theta_min      3.9710
_cell_volume                     2725.23(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  29.00   0.50    0.50    --    0.00 -38.00  60.00   98
  2  \w    -24.00  43.00   0.50    0.50    --    0.00  38.00  60.00  134
  3  \w    -87.00 -62.00   0.50    0.50    --    0.00 -77.00 -60.00   50
  4  \w    -79.00 -40.00   0.50    0.50    --    0.00 -38.00  60.00   78
  5  \w     49.00  88.00   0.50    0.50    --    0.00  38.00  60.00   78
  6  \w    -23.00  35.00   0.50    0.50    --    0.00 -77.00 -60.00  116
  7  \w     85.00 135.00   0.50    0.50    --   97.60 -82.00 -30.00  100
  8  \w     71.00 187.00   0.50    0.50    --   97.60  45.00-150.00  232
  9  \w     31.00  58.00   0.50    0.50    --   97.60 -82.00  90.00   54
 10  \w     81.00 187.00   0.50    0.50    --   97.60  45.00 120.00  212
 11  \w     69.00 169.00   0.50    0.50    --   97.60  45.00 150.00  200
 12  \w     13.00  39.00   0.50    0.50    --   97.60 -82.00 -30.00   52
 13  \w     12.00 131.00   0.50    0.50    --   97.60 -82.00  30.00  238
 14  \w     12.00 115.00   0.50    0.50    --   97.60 -82.00-180.00  206
 15  \w     16.00 135.00   0.50    0.50    --   97.60 -82.00 -90.00  238
 16  \w     67.00 128.00   0.50    0.50    --   97.60 -82.00  90.00  122
 17  \w      8.00 127.00   0.50    0.50    --   97.60 -61.00 -90.00  238
 18  \w     70.00 162.00   0.50    0.50    --   97.60  45.00-120.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0151846000
_diffrn_orient_matrix_UB_12      0.0512050000
_diffrn_orient_matrix_UB_13      -0.0761363000
_diffrn_orient_matrix_UB_21      -0.1376112000
_diffrn_orient_matrix_UB_22      0.0260713000
_diffrn_orient_matrix_UB_23      0.0011577000
_diffrn_orient_matrix_UB_31      0.0303540000
_diffrn_orient_matrix_UB_32      0.0924010000
_diffrn_orient_matrix_UB_33      0.0420449000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22522
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.393
_diffrn_reflns_theta_min         3.996
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.325
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0551
_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^)+(0.1257P)^2^+0.5640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4908
_reflns_number_total             5377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04501b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7126920--7126923.cif.'
_cod_database_code               7126922
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_usercomment     'C H O'
_shelx_estimated_absorpt_t_max   0.133
_shelx_estimated_absorpt_t_min   0.056
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C1(H1A,H1B), C6(H6A,H6B), C7(H7A,H7B), C12(H12A,H12B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              19099
_shelx_hkl_checksum              9668
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.618
_oxdiff_exptl_absorpt_empirical_full_min 0.607