N-Heterocyclic Phosphenium Ligands as Sterically and Electronically-Tunable Isolobal Analogues of Nitrosyls
Baofei Pan; Zhequan Xu; Mark W. Bezpalko; Bruce M. Foxman; Christine M. Thomas; Inorganic Chemistry 51 (2012) 4170–4179; doi:10.1021/ic202581v

data_4328803
_publ_section_title
;
 N-Heterocyclic Phosphenium Ligands as Sterically and
 Electronically-Tunable Isolobal Analogues of Nitrosyls
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4170
_journal_page_last               4179
_journal_paper_doi               10.1021/ic202581v
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H37 Cl2 F6 I1 N2 P4 Pt1'
_chemical_formula_sum            'C40 H37 Cl2 F6 I N2 P4 Pt'
_chemical_formula_weight         1176.53
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             11-10-08
_audit_creation_method           CRYSTALS_ver_14.30
_cell_angle_alpha                90
_cell_angle_beta                 97.486(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0478(5)
_cell_length_b                   10.4295(5)
_cell_length_c                   21.9895(9)
_cell_measurement_reflns_used    5554
_cell_measurement_temperature    120
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2057.33(17)
_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 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.045
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16727
_diffrn_reflns_theta_full        26.474
_diffrn_reflns_theta_max         27.014
_diffrn_reflns_theta_min         1.868
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.507
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.98
_refine_diff_density_min         -4.49
_refine_ls_abs_structure_details 'Flack (1983), 3370 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.188(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0122665
_refine_ls_shift/su_mean         0.0013328
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ +15.62P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1163
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1163
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                6968
_reflns_number_total             7850
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.76
_oxford_diffrn_Wilson_scale      267.43
_oxford_refine_ls_r_factor_ref   0.0587
_oxford_refine_ls_scale          0.066378(12)
_oxford_reflns_number_all        7850
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'BFPAN_125_0m in Pn'
_cod_data_source_file            ic202581v_si_002_11.cif
_cod_data_source_block           17
_cod_original_sg_symbol_H-M      'P 1 n 1 '
_cod_original_formula_sum        'C40 H37 Cl2 F6 I1 N2 P4 Pt1'
_cod_database_code               4328803
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT PT   (    1 ,X'S,U'S)  UNTIL P    (    4 ) 
CONT P    (   20 ,X'S,U[ISO]) 
CONT F    (    1 ,X'S,U'S)  UNTIL C    (   39 ) 
CONT C    (   40 ,X'S,U[ISO])  UNTIL C    (   41 ) 
SUMFIX ELEMENT SCALES 
SUMFIX PART(1001,OCC) AND PART(1002,OCC) 
SUMFIX PART(1003,OCC) AND PART(1004,OCC) 
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   (  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   (  18,X'S) H   ( 181,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   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) H   ( 393,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,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) 
DISTANCE 1.700000 , 0.010000 = N(2) TO P(20) 
U(IJ)'S  0.0, 0.004000 = PT(1) TO P(2) 
U(IJ)'S  0.0, 0.010000 = C(10) TO C(11) 
U(IJ)'S  0.0, 0.010000 = C(11) TO C(12) 
U(IJ)'S  0.0, 0.010000 = P(4) TO F(3) 
U(IJ)'S  0.0, 0.010000 = C(36) TO C(37) 
DISTANCE 1.760000 , 0.020000 = CL(1) TO C(40) 
DISTANCE 1.760000 , 0.020000 = C(41) TO CL(1) 
DISTANCE 1.760000 , 0.020000 = CL(2) TO C(40) 
DISTANCE 1.760000 , 0.015000 = C(41) TO CL(2) 
END                                                                             
;