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_7126920
_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         'C18 H14 O10 P2 W2'
_chemical_formula_sum            'C18 H14 O10 P2 W2'
_chemical_formula_weight         819.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-13
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-04 deposited with the CCDC.	2020-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.4853(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.4396(4)
_cell_length_b                   10.82292(16)
_cell_length_c                   18.9442(3)
_cell_measurement_reflns_used    8342
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.5240
_cell_measurement_theta_min      3.6700
_cell_volume                     4853.47(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -78.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000  -60.0000 66

  2 omega -103.00  -11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000 -150.0000 92

  3 omega  -64.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000  -60.0000 26

  4 omega  -99.00  -74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000  -60.0000 25

  5 omega   -3.00   39.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000    0.0000 42

  6 omega  -29.00    6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -77.0000  -60.0000 35

  7 omega   70.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000 -180.0000 26

  8 omega   42.00   95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000  150.0000 53

  9 omega  -26.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -77.0000   60.0000 54

 10 omega   12.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -120.0000 65

 11 omega   58.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  -60.0000 44

 12 omega   27.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -77.0000  -60.0000 26

 13 omega   40.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -77.0000   60.0000 25

 14 omega   47.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000    0.0000 26

 15 omega   59.00   99.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 40

 16 omega   82.00  176.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 94

 17 omega   46.00   90.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 44

 18 omega   46.00   82.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 36

 19 omega   41.00   96.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 55

 20 omega   54.00   81.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 27

 21 omega  150.00  175.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 25

 22 omega   44.00  109.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  150.0000 65

 23 omega   82.00  134.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 52

 24 omega   56.00   97.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 41

 25 omega   38.00   64.00   1.0000    2.7500
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
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_diffrn_orient_matrix_UB_11      -0.0384086000
_diffrn_orient_matrix_UB_12      -0.0131098000
_diffrn_orient_matrix_UB_13      0.0463435000
_diffrn_orient_matrix_UB_21      0.0521353000
_diffrn_orient_matrix_UB_22      0.0082092000
_diffrn_orient_matrix_UB_23      0.0741241000
_diffrn_orient_matrix_UB_31      -0.0065526000
_diffrn_orient_matrix_UB_32      0.1414721000
_diffrn_orient_matrix_UB_33      0.0000055000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20747
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         3.735
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.960
_exptl_absorpt_correction_T_max  0.260
_exptl_absorpt_correction_T_min  0.071
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_description       prism
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.3321
_exptl_crystal_size_mid          0.1992
_exptl_crystal_size_min          0.1181
_refine_diff_density_max         1.192
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         8648
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0462P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7122
_reflns_number_total             8648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04501b2.cif
_cod_data_source_block           201806279
_cod_depositor_comments
'Adding full bibliography for 7126920--7126923.cif.'
_cod_original_cell_volume        4853.46(15)
_cod_database_code               7126920
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C18H14O10P2W2
_chemical_oxdiff_usercomment     1
_reflns_odcompleteness_completeness 99.95
_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:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C16(H16A,H16B), C11'(H11C,
 H11D), C12'(H12C,H12D), C13'(H13C,H13D), C16'(H16C,H16D)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C17'(H17D,H17E,H17F), C18'(H18D,
 H18E,H18F)
;
_olex2_date_sample_data_collection 2018-06-13
_olex2_submission_special_instructions 'No special instructions were received'