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_4328794
_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         'C49 H57.00 F6 N2 O2.00 P5 Pd1'
_chemical_formula_sum            'C49 H57 F6 N2 O2 P5 Pd'
_chemical_formula_weight         1081.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             11-07-11
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 90.070(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3494(9)
_cell_length_b                   19.5879(13)
_cell_length_c                   16.6704(10)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     4685.6(5)
_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 0.995
_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  0.026
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58569
_diffrn_reflns_theta_full        29.469
_diffrn_reflns_theta_max         30.071
_diffrn_reflns_theta_min         1.604
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       'prism fragment'
_exptl_crystal_F_000             2223.999
_exptl_crystal_size_max          0.648
_exptl_crystal_size_mid          0.538
_exptl_crystal_size_min          0.520
_refine_diff_density_max         0.92
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0375
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         13671
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.0122379
_refine_ls_shift/su_mean         0.0006681
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 4.13P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0812
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0812
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              27
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                13342
_reflns_number_total             13671
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.34
_oxford_diffrn_Wilson_scale      59.96
_oxford_refine_ls_r_factor_ref   0.0312
_oxford_refine_ls_scale          0.054598(5)
_oxford_reflns_number_all        13671
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'bfpan_598_0m in P2(1)/n'
_cod_data_source_file            ic202581v_si_002_02.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C49 H57.00 F6 N2 O2.00 P5 Pd1'
_cod_database_code               4328794
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT PD   (    1 ,X'S,U'S)  UNTIL O    (  1 ) 
CONT O(20, X'S,U[ISO]) UNTIL O(21) 
CONT N(1,X'S,U'S) UNTIL C(45) 
CONT C(460,X'S,U[ISO]) UNTIL C(491) 
SUMFIX ELEMENT SCALES 
SUMFIX PART(1001,OCC) AND PART(1002,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) H   ( 393,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 402,X'S) H   ( 403,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) H   ( 442,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) 
RIDE C   ( 460,X'S) H   (4601,X'S) H   (4602,X'S) 
RIDE C   ( 461,X'S) H   (4611,X'S) H   (4612,X'S) 
RIDE C   ( 470,X'S) H   (4701,X'S) H   (4702,X'S) 
RIDE C   ( 471,X'S) H   (4711,X'S) H   (4712,X'S) 
RIDE C   ( 480,X'S) H   (4801,X'S) H   (4802,X'S) 
RIDE C   ( 481,X'S) H   (4811,X'S) H   (4812,X'S) 
RIDE C   ( 490,X'S) H   (4901,X'S) H   (4902,X'S) 
RIDE C   ( 491,X'S) H   (4911,X'S) H   (4912,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                                                                             
;