The new diphosphanylphosphido complexes of tungsten(vi) and molybdenum(vi). Their synthesis, structures and properties.
Wiśniewska, A; Grubba, R.; Ponikiewski, Ł; Zauliczny, M.; Pikies, J.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10213–10222; doi:10.1039/c8dt01977k

data_7046941
_publ_section_title
;
 The new diphosphanylphosphido complexes of tungsten(vi) and
 molybdenum(vi). Their synthesis, structures and properties.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10213
_journal_page_last               10222
_journal_paper_doi               10.1039/c8dt01977k
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C36 H62 Cl Mo N2 P3'
_chemical_formula_sum            'C36 H62 Cl Mo N2 P3'
_chemical_formula_weight         747.17
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_audit_creation_date             2018-07-02
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5885(16)
_cell_length_b                   20.9626(16)
_cell_length_c                   18.7533(17)
_cell_measurement_reflns_used    4220
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      285386
_cell_measurement_theta_min      2.2287
_cell_measurement_wavelength     0.71073
_cell_volume                     4110.8(8)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
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_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0063275
_diffrn_orient_matrix_UB_12      -0.0264317
_diffrn_orient_matrix_UB_13      0.0239987
_diffrn_orient_matrix_UB_21      0.0023077
_diffrn_orient_matrix_UB_22      0.0211072
_diffrn_orient_matrix_UB_23      0.0297539
_diffrn_orient_matrix_UB_31      -0.0674812
_diffrn_orient_matrix_UB_32      -0.0018205
_diffrn_orient_matrix_UB_33      -0.002761
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17938
_diffrn_reflns_point_group_measured_fraction_full 0.681
_diffrn_reflns_point_group_measured_fraction_max 0.652
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.233
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.91126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.86
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 1766 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     775
_refine_ls_number_reflns         11692
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.298
_reflns_Friedel_fraction_full    0.344
_reflns_Friedel_fraction_max     0.308
_reflns_number_gt                9020
_reflns_number_total             11692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01977k2.cif
_cod_data_source_block           'global_CCDC2'
_cod_depositor_comments
'Adding full bibliography for 7046939--7046943.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7046941
_shelx_estimated_absorpt_t_min   0.88
_shelx_estimated_absorpt_t_max   0.884