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_4328797
_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_formula_moiety         'C21 H20 Cl4.50 N1 P1.50 Pd0.50'
_chemical_formula_sum            'C21 H20 Cl4.5 N P1.5 Pd0.5'
_chemical_formula_weight         545.59
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             11-10-08
_audit_creation_method           CRYSTALS_ver_14.30
_cell_angle_alpha                103.872(4)
_cell_angle_beta                 93.640(4)
_cell_angle_gamma                109.037(3)
_cell_formula_units_Z            4
_cell_length_a                   9.4301(5)
_cell_length_b                   13.3402(7)
_cell_length_c                   20.3562(14)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    120
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     2322.0(2)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_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 0.994
_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  0.056
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42645
_diffrn_reflns_theta_full        26.519
_diffrn_reflns_theta_max         27.061
_diffrn_reflns_theta_min         1.043
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       'acicular fragment'
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.413
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.20
_refine_diff_density_min         -2.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         10129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.0134697
_refine_ls_shift/su_mean         0.0011370
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 8.66P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1520
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1520
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                7554
_reflns_number_total             10129
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.93
_oxford_diffrn_Wilson_scale      49.23
_oxford_refine_ls_r_factor_ref   0.0758
_oxford_refine_ls_scale          0.11455(4)
_oxford_reflns_number_all        10129
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bfpan_18_0ma in P-1'
_cod_data_source_file            ic202581v_si_002_05.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C21 H20 Cl4.50 N1 P1.50 Pd0.50'
_cod_database_code               4328797
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT PD   (    1 ,X'S,U'S)  UNTIL P    (    3 ) 
CONT P    (   20 ,X'S,U[ISO]) 
CONT N    (    1 ,X'S,U'S)  UNTIL C    (   42 ) 
SUMFIX P(2,OCC) AND P(20,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   (  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   (  39,X'S) H   ( 391,X'S) H   ( 392,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) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,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) 
END                                                                             
;