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

data_4123107
_publ_section_title
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 Secondary Phosphinocarbyne and Phosphaisonitrile Complexes.
;
_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         'C24 H34 B1 N6 O2 P1 W1'
_chemical_formula_sum            'C24 H34 B N6 O2 P W'
_chemical_formula_weight         664.21
_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                 104.4069(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6309(2)
_cell_length_b                   14.6523(3)
_cell_length_c                   18.3905(4)
_cell_measurement_reflns_used    247379
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2774.55(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.136
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50004
_diffrn_reflns_theta_full        27.546
_diffrn_reflns_theta_max         27.546
_diffrn_reflns_theta_min         2.676
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.252
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.78
_refine_diff_density_min         -1.49
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9724
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6374
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.0010231
_refine_ls_shift/su_mean         0.0000141
_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: 
 18.4 25.4 12.5 2.98 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1606
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1606
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                4658
_reflns_number_total             6380
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.18
_oxford_diffrn_Wilson_scale      90.36
_oxford_refine_ls_r_factor_ref   0.0909
_oxford_refine_ls_scale          0.14023(9)
_oxford_reflns_number_all        6374
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ja511308k_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C24 H34 B1 N6 O2 P1 W1'
_cod_database_code               4123107
_iucr_refine_instruction_details_constraints
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BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
END                                                                             
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_iucr_refine_instruction_details_restraints
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REM NO H   NO #H U MULT DIST 
REM C-H 
REM >4           1.5    .96 DISORDER 
REM 1      1     1.2    .93 C C-H (ACETYLENE) 
REM 1      2     1.2    .93 C-C(H)-C 
REM 1      3     1.2    .98 (C)3-C-H 
REM 2      1     1.2    .93 C=C-H(2) 
REM 2      2     1.2    .97 (C)2-C-(H)2 
REM 3      1     1.5    .96 C-C-(H)3 
REM N-H 
REM >4           1.5    .89 DISORDER 
REM 1      1     1.2    .86 N-N/H 
REM 1      2     1.2    .86 (C)2-N-H 
REM 1      3     1.2    .89 (C)3-N-H 
REM 2      1     1.2    .86 C-N-(H)2 
REM 2      2     1.2    .89 (C)2-N-(H)2 
REM 3      1     1.2    .89 C-H-(H)3 
REM O-H 
REM 1      1     1.5    .82 O-H 
REM 
REM DIST      ESD = 0.02 
REM VIB       ESD = 0.002 
REM ANGLE     ESD = 2.0 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 11) TO H(113) 
CONT C ( 11) TO H(111) 
CONT C ( 11) TO H(112) 
REST 0.083, 0.002 = H(113,U[ISO]) 
REST 0.083, 0.002 = H(111,U[ISO]) 
REST 0.083, 0.002 = H(112,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(12) TO C ( 11) TO H(113) 
CONT C(12) TO C ( 11) TO H(111) 
CONT C(12) TO C ( 11) TO H(112) 
ANGLE 0.0, 2.0 = MEAN H(113) TO C ( 11) TO H(111) 
CONT H(113) TO C ( 11) TO H(112) 
CONT H(111) TO C ( 11) TO H(112) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 13) TO H(131) 
REST 0.066, 0.002 = H(131,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(131) TO C ( 13) TO C(12) 
CONT H(131) TO C ( 13) TO C(14) 
PLANAR C ( 13) C(12) C(14) H(131) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 15) TO H(153) 
CONT C ( 15) TO H(151) 
CONT C ( 15) TO H(152) 
REST 0.100, 0.002 = H(153,U[ISO]) 
REST 0.100, 0.002 = H(151,U[ISO]) 
REST 0.100, 0.002 = H(152,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(14) TO C ( 15) TO H(153) 
CONT C(14) TO C ( 15) TO H(151) 
CONT C(14) TO C ( 15) TO H(152) 
ANGLE 0.0, 2.0 = MEAN H(153) TO C ( 15) TO H(151) 
CONT H(153) TO C ( 15) TO H(152) 
CONT H(151) TO C ( 15) TO H(152) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 21) TO H(211) 
CONT C ( 21) TO H(213) 
CONT C ( 21) TO H(212) 
REST 0.071, 0.002 = H(211,U[ISO]) 
REST 0.071, 0.002 = H(213,U[ISO]) 
REST 0.071, 0.002 = H(212,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(22) TO C ( 21) TO H(211) 
CONT C(22) TO C ( 21) TO H(213) 
CONT C(22) TO C ( 21) TO H(212) 
ANGLE 0.0, 2.0 = MEAN H(211) TO C ( 21) TO H(213) 
CONT H(211) TO C ( 21) TO H(212) 
CONT H(213) TO C ( 21) TO H(212) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 23) TO H(231) 
REST 0.041, 0.002 = H(231,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(231) TO C ( 23) TO C(22) 
CONT H(231) TO C ( 23) TO C(24) 
PLANAR C ( 23) C(22) C(24) H(231) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 25) TO H(251) 
CONT C ( 25) TO H(253) 
CONT C ( 25) TO H(252) 
REST 0.083, 0.002 = H(251,U[ISO]) 
REST 0.083, 0.002 = H(253,U[ISO]) 
REST 0.083, 0.002 = H(252,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(24) TO C ( 25) TO H(251) 
CONT C(24) TO C ( 25) TO H(253) 
CONT C(24) TO C ( 25) TO H(252) 
ANGLE 0.0, 2.0 = MEAN H(251) TO C ( 25) TO H(253) 
CONT H(251) TO C ( 25) TO H(252) 
CONT H(253) TO C ( 25) TO H(252) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 31) TO H(312) 
CONT C ( 31) TO H(311) 
CONT C ( 31) TO H(313) 
REST 0.074, 0.002 = H(312,U[ISO]) 
REST 0.074, 0.002 = H(311,U[ISO]) 
REST 0.074, 0.002 = H(313,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(32) TO C ( 31) TO H(312) 
CONT C(32) TO C ( 31) TO H(311) 
CONT C(32) TO C ( 31) TO H(313) 
ANGLE 0.0, 2.0 = MEAN H(312) TO C ( 31) TO H(311) 
CONT H(312) TO C ( 31) TO H(313) 
CONT H(311) TO C ( 31) TO H(313) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 33) TO H(331) 
REST 0.046, 0.002 = H(331,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(331) TO C ( 33) TO C(32) 
CONT H(331) TO C ( 33) TO C(34) 
PLANAR C ( 33) C(32) C(34) H(331) 
REM            3 H ON SP 3 
DIST 0.96, 0.02 = 
CONT C ( 35) TO H(352) 
CONT C ( 35) TO H(353) 
CONT C ( 35) TO H(351) 
REST 0.087, 0.002 = H(352,U[ISO]) 
REST 0.087, 0.002 = H(353,U[ISO]) 
REST 0.087, 0.002 = H(351,U[ISO]) 
ANGLE 109.54, 2.0 = 
CONT C(34) TO C ( 35) TO H(352) 
CONT C(34) TO C ( 35) TO H(353) 
CONT C(34) TO C ( 35) TO H(351) 
ANGLE 0.0, 2.0 = MEAN H(352) TO C ( 35) TO H(353) 
CONT H(352) TO C ( 35) TO H(351) 
CONT H(353) TO C ( 35) TO H(351) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 41) TO H(411) 
REST 0.057, 0.002 = H(411,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(411) TO C ( 41) TO P(1) 
CONT H(411) TO C ( 41) TO C(42) 
CONT H(411) TO C ( 41) TO C(46) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 42) TO H(421) 
CONT C ( 42) TO H(422) 
REST 0.074, 0.002 = H(421,U[ISO]) 
REST 0.074, 0.002 = H(422,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(421) TO C ( 42) TO C(41) 
CONT H(421) TO C ( 42) TO C(43) 
CONT H(422) TO C ( 42) TO C(41) 
CONT H(422) TO C ( 42) TO C(43) 
ANGLE 109.54, 2.0 = 
CONT H(421) TO C ( 42) TO H(422) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 43) TO H(431) 
CONT C ( 43) TO H(432) 
REST 0.110, 0.002 = H(431,U[ISO]) 
REST 0.110, 0.002 = H(432,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(431) TO C ( 43) TO C(42) 
CONT H(431) TO C ( 43) TO C(44) 
CONT H(432) TO C ( 43) TO C(42) 
CONT H(432) TO C ( 43) TO C(44) 
ANGLE 109.54, 2.0 = 
CONT H(431) TO C ( 43) TO H(432) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 44) TO H(441) 
CONT C ( 44) TO H(442) 
REST 0.105, 0.002 = H(441,U[ISO]) 
REST 0.105, 0.002 = H(442,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(441) TO C ( 44) TO C(43) 
CONT H(441) TO C ( 44) TO C(45) 
CONT H(442) TO C ( 44) TO C(43) 
CONT H(442) TO C ( 44) TO C(45) 
ANGLE 109.54, 2.0 = 
CONT H(441) TO C ( 44) TO H(442) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 45) TO H(451) 
CONT C ( 45) TO H(452) 
REST 0.107, 0.002 = H(451,U[ISO]) 
REST 0.107, 0.002 = H(452,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(451) TO C ( 45) TO C(44) 
CONT H(451) TO C ( 45) TO C(46) 
CONT H(452) TO C ( 45) TO C(44) 
CONT H(452) TO C ( 45) TO C(46) 
ANGLE 109.54, 2.0 = 
CONT H(451) TO C ( 45) TO H(452) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 46) TO H(461) 
CONT C ( 46) TO H(462) 
REST 0.074, 0.002 = H(461,U[ISO]) 
REST 0.074, 0.002 = H(462,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(461) TO C ( 46) TO C(45) 
CONT H(461) TO C ( 46) TO C(41) 
CONT H(462) TO C ( 46) TO C(45) 
CONT H(462) TO C ( 46) TO C(41) 
ANGLE 109.54, 2.0 = 
CONT H(461) TO C ( 46) TO H(462) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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