New 10-Membered Inorganic Heterocyclic Diphosphanes, PhN(PX)2{(-OC6H2(tBu)2)(μ-S)((tBu)2C6H2O-)} (X = Cl, F). Synthesis and Transition Metal Complexes (Molybdenum(0), Ruthenium(II), Palladium(II), and Platinum(II)) of Heterocyclic Diphosphanes. Crystal and Molecular Structures of the Chloro Derivative, PhN(PCl)2{(-OC6H2(tBu)2)(μ-S)((tBu)2C6H2O-)}, and of a Molybdenum(0) Complex of the Fluoro Derivative, [Mo(CO)3{η3-PhN(PF)2{(-OC6H2(tBu)2)(μ-S)((tBu)2C6H2O-)}-κP,κP,κS}]
Maravanji S. Balakrishna; Rashmishree Panda; Joel T. Mague; Inorganic Chemistry 40 (2001) 5620–5625; doi:10.1021/ic010518j

data_4320434
_publ_section_title
;
 New 10-Membered Inorganic Heterocyclic Diphosphanes,
 PhN(PX)2{(-OC6H2(tBu)2)(\m-S)((tBu)2C6H2O-)} (X = Cl, F). Synthesis and
 Transition Metal Complexes (Molybdenum(0), Ruthenium(II), Palladium(II),
 and Platinum(II)) of Heterocyclic Diphosphanes. Crystal and Molecular
 Structures of the Chloro Derivative,
 PhN(PCl)2{(-OC6H2(tBu)2)(\m-S)((tBu)2C6H2O-)}, and of a Molybdenum(0)
 Complex of the Fluoro Derivative,
 [Mo(CO)3{\h3-PhN(PF)2{(-OC6H2(tBu)2)(\m-S)((tBu)2C6H2O-)}-\kP,\kP,\kS}]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5620
_journal_page_last               5625
_journal_paper_doi               10.1021/ic010518j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C37 H45 F2 Mo N O5 P2 S'
_chemical_formula_weight         811.68
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.382(4)
_cell_angle_beta                 98.894(5)
_cell_angle_gamma                114.284(4)
_cell_formula_units_Z            2
_cell_length_a                   11.7037(7)
_cell_length_b                   12.2971(5)
_cell_length_c                   16.5033(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.40
_cell_measurement_theta_min      15.98
_cell_volume                     2034.5(2)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1987)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1997)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8371
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        8.2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.8927
_exptl_absorpt_correction_T_min  0.8327
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scan (North, et al., 1968)'
_exptl_crystal_colour            Amber
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.3386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                5094
_reflns_number_total             7963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010518j_2.cif
_cod_data_source_block           msb07
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2034.51(18)
_cod_database_code               4320434