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_7046942
_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_formula_moiety         'C40 H72 Cl Mo N4 P3'
_chemical_formula_sum            'C40 H72 Cl Mo N4 P3'
_chemical_formula_weight         833.31
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-07-03
_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                105.878(5)
_cell_angle_beta                 102.963(6)
_cell_angle_gamma                102.300(7)
_cell_formula_units_Z            4
_cell_length_a                   11.0012(10)
_cell_length_b                   20.8791(14)
_cell_length_c                   22.0534(14)
_cell_measurement_reflns_used    28474
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      3.55
_cell_measurement_wavelength     0.71073
_cell_volume                     4540.1(7)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area X-Red32 1.63.4.0 (STOE, 2017) 
;
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      ' 217 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.036
_diffrn_reflns_Laue_measured_fraction_full 0.98
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40229
_diffrn_reflns_point_group_measured_fraction_full 0.98
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         3.041
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.973
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     901
_refine_ls_number_reflns         21582
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0597P)^2^+4.1319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0
_reflns_number_gt                17464
_reflns_number_total             21582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01977k2.cif
_cod_data_source_block           'global_CCDC3'
_cod_depositor_comments
'Adding full bibliography for 7046939--7046943.cif.'
_cod_original_cell_volume        4540.1(6)
_cod_database_code               7046942
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.901