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_7126923
_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         'C32 H40 Mo2 O8 P4'
_chemical_formula_sum            'C32 H40 Mo2 O8 P4'
_chemical_formula_weight         868.40
_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             2018-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-05 deposited with the CCDC.	2020-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                87.053(3)
_cell_angle_beta                 85.059(3)
_cell_angle_gamma                74.342(3)
_cell_formula_units_Z            4
_cell_length_a                   12.1297(4)
_cell_length_b                   17.3992(6)
_cell_length_c                   18.9772(7)
_cell_measurement_reflns_used    10691
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.9140
_cell_measurement_theta_min      3.4670
_cell_volume                     3840.5(2)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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  -90.00  -64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000    0.0000 26

  2 omega  -76.00  -32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000  120.0000 44

  3 omega -101.00  -55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000   90.0000 46

  4 omega  -40.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -37.0000   90.0000 26

  5 omega -104.00  -78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000  120.0000 26

  6 omega   60.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  -90.0000 48

  7 omega    8.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   60.0000 60

  8 omega   70.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000   30.0000 26

  9 omega    8.00   52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -60.0000 44

 10 omega    9.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  -90.0000 96

 11 omega   18.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000  150.0000 28

 12 omega  -14.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -57.0000  -30.0000 47

 13 omega   71.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   60.0000 35

 14 omega   27.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  150.0000 79

 15 omega   -3.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -30.0000 75

 16 omega   35.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   30.0000 68

 17 omega   18.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000   30.0000 59

 18 omega   -2.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -90.0000 55

 19 omega   48.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  150.0000 27

 20 omega   19.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -150.0000 41

 21 omega   53.00   90.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 37

 22 omega   72.00  109.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 37

 23 omega   92.00  176.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 84

 24 omega   54.00  112.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 58

 25 omega   59.00   96.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -150.0000 37

 26 omega   62.00  103.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 41

 27 omega   45.00   89.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 44

 28 omega   46.00   87.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 41

 29 omega   67.00  108.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -150.0000 41

 30 omega  119.00  174.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -150.0000 55

 31 omega   43.00   84.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 41

 32 omega   42.00  127.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 85

 33 omega  149.00  175.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 26

 34 omega   93.00  125.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -150.0000 32

 35 omega   41.00   66.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -150.0000 25

 36 omega   63.00   97.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 34

 37 omega   38.00  109.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 71

 38 omega   38.00   77.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 39

 39 omega   39.00  113.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -150.0000 74

 40 omega   98.00  178.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   90.0000 80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0557171000
_diffrn_orient_matrix_UB_12      -0.0322500000
_diffrn_orient_matrix_UB_13      0.0692930000
_diffrn_orient_matrix_UB_21      -0.0293284000
_diffrn_orient_matrix_UB_22      0.0856704000
_diffrn_orient_matrix_UB_23      0.0270687000
_diffrn_orient_matrix_UB_31      -0.1163290000
_diffrn_orient_matrix_UB_32      -0.0091350000
_diffrn_orient_matrix_UB_33      0.0333298000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30703
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.475
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.296
_exptl_absorpt_correction_T_max  0.415
_exptl_absorpt_correction_T_min  0.257
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.2783
_exptl_crystal_size_mid          0.2328
_exptl_crystal_size_min          0.2024
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00101(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         13720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10795
_reflns_number_total             13720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04501b2.cif
_cod_data_source_block           201808353
_cod_depositor_comments
'Adding full bibliography for 7126920--7126923.cif.'
_cod_database_code               7126923
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C32H15O8N2Mo2P4
_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:
 C9(H9A,H9B), C12(H12A,H12B), C15(H15A,H15B), C18(H18A,H18B), C21(H21A,H21B),
 C24(H24A,H24B), C27(H27A,H27B), C30(H30A,H30B), C9'(H9'A,H9'B), C12'(H12C,
 H12D), C15'(H15C,H15D), C18'(H18C,H18D), C21'(H21C,H21D), C24'(H24C,H24D),
 C27'(H27C,H27D), C30'(H30C,H30D)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C13'(H13D,H13E,H13F), C14'(H14D,H14E,H14F), C19'(H19D,H19E,H19F),
 C20'(H20D,H20E,H20F), C25'(H25D,H25E,H25F), C26'(H26D,H26E,H26F), C31'(H31D,
 H31E,H31F), C32'(H32D,H32E,H32F)
;
_olex2_submission_special_instructions 'No special instructions were received'