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_4320433
_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            'C34 H45 Cl2 N O2 P2 S'
_chemical_formula_weight         664.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.918(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8492(8)
_cell_length_b                   17.6284(19)
_cell_length_c                   21.2737(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.35
_cell_measurement_theta_min      14.97
_cell_volume                     3600.2(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.1286
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6782
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        8.0
_diffrn_standards_interval_count 2
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1772
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+0.3297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1585
_reflns_number_gt                3108
_reflns_number_total             6384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010518j_1.cif
_cod_data_source_block           MSB06
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4320433