Heterolytic addition of E-H bonds across Pt-P bonds in Pt N-heterocyclic phosphenium/phosphido complexes.
Pan, Baofei; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9083–9090; doi:10.1039/c2dt30455d

data_7019763
_publ_section_title
;
 Heterolytic addition of E-H bonds across Pt-P bonds in Pt N-heterocyclic
 phosphenium/phosphido complexes.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9083
_journal_page_last               9090
_journal_paper_doi               10.1039/c2dt30455d
_journal_volume                  41
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H32 Cl N2 P3 Pt, F6 P'
_chemical_formula_sum            'C38 H32 Cl F6 N2 P4 Pt'
_chemical_formula_weight         985.11
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-02-16
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 98.743(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1189(4)
_cell_length_b                   13.4744(5)
_cell_length_c                   22.8621(9)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     3689.9(2)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21159
_diffrn_reflns_theta_full        30.046
_diffrn_reflns_theta_max         30.046
_diffrn_reflns_theta_min         1.700
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.111
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.16
_refine_diff_density_min         -2.13
_refine_ls_abs_structure_details 'Flack (1983), 9983 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.500(7)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9786
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         21159
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.0061564
_refine_ls_shift/su_mean         0.0001530
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 6.59P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0835
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0835
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                17543
_reflns_number_total             21159
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0552
_oxford_refine_ls_scale          0.074091(6)
_oxford_reflns_number_all        21159
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bfpan_740_0m in P2(1)/n'
_cod_data_source_file            c2dt30455d.txt
_cod_data_source_block           6PF6
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C38 H32 Cl1 F6.00 N2 P4 Pt1'
_cod_database_code               7019763
_iucr_refine_instruction_details_constraints
;
BLOCK
CONT SCALE
CONT PT ( 1 ,X'S,U'S) UNTIL F ( 1 )
CONT F ( 2 ,X'S,U[ISO]) UNTIL F ( 5 )
CONT F ( 6 ,X'S,U'S)
CONT F ( 21 ,X'S,U[ISO]) UNTIL F ( 24 )
CONT F ( 101 ,X'S,U'S)
CONT F ( 102 ,X'S,U[ISO]) UNTIL F ( 105 )
CONT F ( 106 ,X'S,U'S)
CONT F ( 121 ,X'S,U[ISO]) UNTIL F ( 124 )
CONT N ( 1 ,X'S,U'S) UNTIL C ( 138 )
SUMFIX P(2,OCC) AND P(3,OCC)
SUMFIX P(102,OCC) AND P(103,OCC)
SUMFIX PART(1001,OCC) AND PART(1002,OCC)
SUMFIX PART(1003,OCC) AND PART(1004,OCC)
SUMFIX ELEMENT SCALES
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
RIDE C ( 102,X'S) H (1021,X'S)
RIDE C ( 103,X'S) H (1031,X'S)
RIDE C ( 104,X'S) H (1041,X'S)
RIDE C ( 105,X'S) H (1051,X'S)
RIDE C ( 106,X'S) H (1061,X'S)
RIDE C ( 108,X'S) H (1081,X'S)
RIDE C ( 109,X'S) H (1091,X'S)
RIDE C ( 110,X'S) H (1101,X'S)
RIDE C ( 111,X'S) H (1111,X'S)
RIDE C ( 112,X'S) H (1121,X'S)
RIDE C ( 114,X'S) H (1141,X'S)
RIDE C ( 115,X'S) H (1151,X'S)
RIDE C ( 116,X'S) H (1161,X'S)
RIDE C ( 117,X'S) H (1171,X'S)
RIDE C ( 119,X'S) H (1191,X'S) H (1192,X'S)
RIDE C ( 120,X'S) H (1201,X'S) H (1202,X'S)
RIDE C ( 122,X'S) H (1221,X'S)
RIDE C ( 123,X'S) H (1231,X'S)
RIDE C ( 124,X'S) H (1241,X'S)
RIDE C ( 125,X'S) H (1251,X'S)
RIDE C ( 128,X'S) H (1281,X'S)
RIDE C ( 129,X'S) H (1291,X'S)
RIDE C ( 130,X'S) H (1301,X'S)
RIDE C ( 131,X'S) H (1311,X'S)
RIDE C ( 132,X'S) H (1321,X'S)
RIDE C ( 134,X'S) H (1341,X'S)
RIDE C ( 135,X'S) H (1351,X'S)
RIDE C ( 136,X'S) H (1361,X'S)
RIDE C ( 137,X'S) H (1371,X'S)
RIDE C ( 138,X'S) H (1381,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
A-U(IJ)'S 0.0, 0.0030000 = P(2) TO P(3)
END
;