The chemistry of parent phosphiranide in the coordination sphere of tungsten.
Hao, Yanwei; Zhang, Chunli; Mei, Yanbo; Tian, Rongqiang; Duan, Zheng; Mathey, François; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8284–8290; doi:10.1039/c6dt00964f

data_7038995
_publ_section_title
;
 The chemistry of parent phosphiranide in the coordination sphere of
 tungsten.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8284
_journal_page_last               8290
_journal_paper_doi               10.1039/c6dt00964f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C20 H13 O10 P3 W2'
_chemical_formula_sum            'C20 H13 O10 P3 W2'
_chemical_formula_weight         873.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-31
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-19 deposited with the CCDC.
2016-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9576(3)
_cell_length_b                   13.0301(3)
_cell_length_c                   29.3579(9)
_cell_measurement_reflns_used    5590
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.7480
_cell_measurement_theta_min      3.4970
_cell_volume                     5339.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -58.00  -33.00   0.5000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  107.0000    9.0000 50

  2 omega  -18.00    7.00   0.5000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104 -107.0000  -88.0000 50

  3 omega   38.00   65.00   0.5000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885 -107.0000  -88.0000 54

  4 omega  -82.00    4.00   0.5000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  -57.0000 -180.0000 172

  5 omega   35.00   96.00   0.5000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000  -90.0000 122

  6 omega   70.00   96.00   0.5000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000  -60.0000 52

  7 omega   44.00   70.00   0.5000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7885  178.0000 -180.0000 52
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0064402000
_diffrn_orient_matrix_UB_12      -0.0352551000
_diffrn_orient_matrix_UB_13      -0.0181563000
_diffrn_orient_matrix_UB_21      0.0113469000
_diffrn_orient_matrix_UB_22      -0.0411916000
_diffrn_orient_matrix_UB_23      0.0148450000
_diffrn_orient_matrix_UB_31      -0.0491123000
_diffrn_orient_matrix_UB_32      -0.0048715000
_diffrn_orient_matrix_UB_33      0.0058073000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25811
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.984
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.174
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.687
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0288P)^2^+4.1721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4374
_reflns_number_total             5453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00964f2.cif
_cod_data_source_block           20150354
_cod_depositor_comments          'Adding full bibliography for 7038995.cif.'
_cod_database_code               7038995
_chemical_oxdiff_formula         C20H20N4O4P1W2
_shelx_estimated_absorpt_t_max   0.393
_shelx_estimated_absorpt_t_min   0.247
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              30287
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'