Secondary Phosphinocarbyne and Phosphaisonitrile Complexes.
Colebatch, Annie L.; Hill, Anthony F.; Journal of the American Chemical Society  (2014) 141208061520004–; doi:10.1021/ja511308k

data_4123108
_publ_section_title
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 Secondary Phosphinocarbyne and Phosphaisonitrile Complexes.
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141208061520004
_journal_paper_doi               10.1021/ja511308k
_journal_year                    2014
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C42 H63 B1 K1 N8 O8 P1 W1'
_chemical_formula_sum            'C42 H63 B K N8 O8 P W'
_chemical_formula_weight         1072.74
_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
_cell_angle_alpha                90
_cell_angle_beta                 95.3960(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6929(3)
_cell_length_b                   23.4328(5)
_cell_length_c                   15.9038(3)
_cell_measurement_reflns_used    18841
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     5451.35(19)
_computing_cell_refinement       'CrysAlis, (Agilent Technologies, 2013)'
_computing_data_collection       'SuperNova, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis, (Agilent Technologies, 2013)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'
_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      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            47041
_diffrn_reflns_theta_full        69.968
_diffrn_reflns_theta_max         72.157
_diffrn_reflns_theta_min         3.369
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.302
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Agilent Technologies, 2013)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;

;
_refine_diff_density_max         1.98
_refine_diff_density_min         -2.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9562
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10633
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.0012404
_refine_ls_shift/su_mean         0.0000212
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.209E+04 0.326E+04 0.181E+04 703. 196. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1122
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1120
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                9566
_reflns_number_total             10683
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.59
_oxford_diffrn_Wilson_scale      0.20
_oxford_refine_ls_r_factor_ref   0.0664
_oxford_refine_ls_scale          2.462(12)
_oxford_reflns_number_all        10638
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            ja511308k_si_001.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C42 H63 B1 K1 N8 O8 P1 W1'
_cod_database_code               4123108
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 153,X'S) H   ( 152,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 253,X'S) H   ( 252,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) H   (1012,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) H   (1022,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) H   (1032,X'S) 
RIDE C   ( 104,X'S) H   (1042,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) H   (1052,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) H   (1062,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) H   (1072,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) H   (1082,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) H   (1092,X'S) 
RIDE C   ( 110,X'S) H   (1102,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1112,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1122,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1132,X'S) 
RIDE C   ( 114,X'S) H   (1142,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) H   (1152,X'S) 
RIDE C   ( 116,X'S) H   (1162,X'S) H   (1161,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) H   (1172,X'S) 
RIDE C   ( 118,X'S) H   (1181,X'S) H   (1182,X'S) 
RIDE B   (   1,X'S) H   (  11,X'S) 
END                                                                             
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_iucr_refine_instructions_details_restraints
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NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.005 = C(101) TO N(101) 
U(IJ) 0.0, 0.005 = C(103) TO O(101) 
U(IJ) 0.0, 0.005 = C(104) TO C(103) 
U(IJ) 0.0, 0.005 = O(102) TO C(104) 
U(IJ) 0.0, 0.005 = C(105) TO O(102) 
U(IJ) 0.0, 0.005 = C(106) TO C(105) 
U(IJ) 0.0, 0.005 = C(118) TO C(117) 
U(IJ) 0.0, 0.005 = C(102) TO C(101) 
U(IJ) 0.0, 0.005 = N(102) TO C(106) 
VIBR 0.0, 0.005 = C(102) TO C(101), C(102) TO O(101) 
VIBR 0.0, 0.005 = O(101) TO C(102), O(101) TO C(103) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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