Synthetic and Structural Studies of Phosphine Coordinated Boronium Salts
Hill, Anthony; Ward, Jas S.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01023K

data_7043012
_publ_section_title
;
 Synthetic and Structural Studies of Phosphine Coordinated Boronium Salts
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01023K
_journal_year                    2017
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C26 H50 B1 P2, H1 B1 Br3'
_chemical_formula_sum            'C26 H51 B2 Br3 P2'
_chemical_formula_weight         686.97
_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_update_record
;
2013-06-07 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2547(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.13810(10)
_cell_length_b                   12.5367(2)
_cell_length_c                   22.3536(3)
_cell_measurement_reflns_used    49823
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     3096.36(7)
_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 (Farrugia, 1997)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.065
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62272
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         3.199
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.026
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.347
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.85
_refine_diff_density_min         -2.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9925
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7079
_refine_ls_number_restraints     176
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.0013843
_refine_ls_shift/su_mean         0.0000418
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 5.05P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1251
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1251
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                5874
_reflns_number_total             7097
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.25
_oxford_diffrn_Wilson_scale      9.56
_oxford_refine_ls_r_factor_ref   0.0549
_oxford_refine_ls_scale          0.4250(6)
_oxford_reflns_number_all        7079
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c7dt01023k2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7043012
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT B    (    1 ,X'S,U'S)  UNTIL C    (   46 ) 
CONT H    (    1 ,X'S)  UNTIL H    (    3 ) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
ANGLE 0.0, 3. = MEAN BR(1) TO B(2) TO H(3), BR(2) TO B(2) TO H(3) 
ANGLE 0.0, 3. = MEAN BR(3) TO B(2) TO H(3), BR(1) TO B(2) TO H(3) 
ANGLE 0.0, 3. = MEAN BR(2) TO B(2) TO H(3), BR(3) TO B(2) TO H(3) 
REM DIST 1.04, 0.03 = B(1) TO H(1) 
REM DIST 1.04, 0.03 = B(1) TO H(2) 
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            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 1) TO H(12) 
CONT C ( 1) TO H(11) 
REST 0.034, 0.002 = H(12,U[ISO]) 
REST 0.034, 0.002 = H(11,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(12) TO C ( 1) TO P(1) 
CONT H(12) TO C ( 1) TO C(2) 
CONT H(11) TO C ( 1) TO P(1) 
CONT H(11) TO C ( 1) TO C(2) 
ANGLE 109.54, 2.0 = 
CONT H(12) TO C ( 1) TO H(11) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 2) TO H(21) 
CONT C ( 2) TO H(22) 
REST 0.034, 0.002 = H(21,U[ISO]) 
REST 0.034, 0.002 = H(22,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(21) TO C ( 2) TO C(1) 
CONT H(21) TO C ( 2) TO P(2) 
CONT H(22) TO C ( 2) TO C(1) 
CONT H(22) TO C ( 2) TO P(2) 
ANGLE 109.54, 2.0 = 
CONT H(21) TO C ( 2) TO H(22) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 11) TO H(111) 
REST 0.029, 0.002 = H(111,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(111) TO C ( 11) TO P(1) 
CONT H(111) TO C ( 11) TO C(12) 
CONT H(111) TO C ( 11) TO C(16) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 12) TO H(121) 
CONT C ( 12) TO H(122) 
REST 0.040, 0.002 = H(121,U[ISO]) 
REST 0.040, 0.002 = H(122,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(121) TO C ( 12) TO C(11) 
CONT H(121) TO C ( 12) TO C(13) 
CONT H(122) TO C ( 12) TO C(11) 
CONT H(122) TO C ( 12) TO C(13) 
ANGLE 109.54, 2.0 = 
CONT H(121) TO C ( 12) TO H(122) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 13) TO H(131) 
CONT C ( 13) TO H(132) 
REST 0.049, 0.002 = H(131,U[ISO]) 
REST 0.049, 0.002 = H(132,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) 
CONT H(132) TO C ( 13) TO C(12) 
CONT H(132) TO C ( 13) TO C(14) 
ANGLE 109.54, 2.0 = 
CONT H(131) TO C ( 13) TO H(132) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 14) TO H(142) 
CONT C ( 14) TO H(141) 
REST 0.046, 0.002 = H(142,U[ISO]) 
REST 0.046, 0.002 = H(141,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(142) TO C ( 14) TO C(13) 
CONT H(142) TO C ( 14) TO C(15) 
CONT H(141) TO C ( 14) TO C(13) 
CONT H(141) TO C ( 14) TO C(15) 
ANGLE 109.54, 2.0 = 
CONT H(142) TO C ( 14) TO H(141) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 15) TO H(151) 
CONT C ( 15) TO H(152) 
REST 0.042, 0.002 = H(151,U[ISO]) 
REST 0.042, 0.002 = H(152,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(151) TO C ( 15) TO C(14) 
CONT H(151) TO C ( 15) TO C(16) 
CONT H(152) TO C ( 15) TO C(14) 
CONT H(152) TO C ( 15) TO C(16) 
ANGLE 109.54, 2.0 = 
CONT H(151) TO C ( 15) TO H(152) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 16) TO H(161) 
CONT C ( 16) TO H(162) 
REST 0.042, 0.002 = H(161,U[ISO]) 
REST 0.042, 0.002 = H(162,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(161) TO C ( 16) TO C(11) 
CONT H(161) TO C ( 16) TO C(15) 
CONT H(162) TO C ( 16) TO C(11) 
CONT H(162) TO C ( 16) TO C(15) 
ANGLE 109.54, 2.0 = 
CONT H(161) TO C ( 16) TO H(162) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 21) TO H(211) 
REST 0.032, 0.002 = H(211,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(211) TO C ( 21) TO P(1) 
CONT H(211) TO C ( 21) TO C(22) 
CONT H(211) TO C ( 21) TO C(26) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 22) TO H(221) 
CONT C ( 22) TO H(222) 
REST 0.046, 0.002 = H(221,U[ISO]) 
REST 0.046, 0.002 = H(222,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(221) TO C ( 22) TO C(21) 
CONT H(221) TO C ( 22) TO C(23) 
CONT H(222) TO C ( 22) TO C(21) 
CONT H(222) TO C ( 22) TO C(23) 
ANGLE 109.54, 2.0 = 
CONT H(221) TO C ( 22) TO H(222) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 23) TO H(232) 
CONT C ( 23) TO H(231) 
REST 0.051, 0.002 = H(232,U[ISO]) 
REST 0.051, 0.002 = H(231,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(232) TO C ( 23) TO C(22) 
CONT H(232) TO C ( 23) TO C(24) 
CONT H(231) TO C ( 23) TO C(22) 
CONT H(231) TO C ( 23) TO C(24) 
ANGLE 109.54, 2.0 = 
CONT H(232) TO C ( 23) TO H(231) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 24) TO H(241) 
CONT C ( 24) TO H(242) 
REST 0.046, 0.002 = H(241,U[ISO]) 
REST 0.046, 0.002 = H(242,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(241) TO C ( 24) TO C(23) 
CONT H(241) TO C ( 24) TO C(25) 
CONT H(242) TO C ( 24) TO C(23) 
CONT H(242) TO C ( 24) TO C(25) 
ANGLE 109.54, 2.0 = 
CONT H(241) TO C ( 24) TO H(242) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 25) TO H(251) 
CONT C ( 25) TO H(252) 
REST 0.047, 0.002 = H(251,U[ISO]) 
REST 0.047, 0.002 = H(252,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(251) TO C ( 25) TO C(24) 
CONT H(251) TO C ( 25) TO C(26) 
CONT H(252) TO C ( 25) TO C(24) 
CONT H(252) TO C ( 25) TO C(26) 
ANGLE 109.54, 2.0 = 
CONT H(251) TO C ( 25) TO H(252) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 26) TO H(261) 
CONT C ( 26) TO H(262) 
REST 0.041, 0.002 = H(261,U[ISO]) 
REST 0.041, 0.002 = H(262,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(261) TO C ( 26) TO C(25) 
CONT H(261) TO C ( 26) TO C(21) 
CONT H(262) TO C ( 26) TO C(25) 
CONT H(262) TO C ( 26) TO C(21) 
ANGLE 109.54, 2.0 = 
CONT H(261) TO C ( 26) TO H(262) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 31) TO H(311) 
REST 0.031, 0.002 = H(311,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(311) TO C ( 31) TO P(2) 
CONT H(311) TO C ( 31) TO C(32) 
CONT H(311) TO C ( 31) TO C(36) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 32) TO H(321) 
CONT C ( 32) TO H(322) 
REST 0.043, 0.002 = H(321,U[ISO]) 
REST 0.043, 0.002 = H(322,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(321) TO C ( 32) TO C(31) 
CONT H(321) TO C ( 32) TO C(33) 
CONT H(322) TO C ( 32) TO C(31) 
CONT H(322) TO C ( 32) TO C(33) 
ANGLE 109.54, 2.0 = 
CONT H(321) TO C ( 32) TO H(322) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 33) TO H(331) 
CONT C ( 33) TO H(332) 
REST 0.048, 0.002 = H(331,U[ISO]) 
REST 0.048, 0.002 = H(332,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) 
CONT H(332) TO C ( 33) TO C(32) 
CONT H(332) TO C ( 33) TO C(34) 
ANGLE 109.54, 2.0 = 
CONT H(331) TO C ( 33) TO H(332) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 34) TO H(342) 
CONT C ( 34) TO H(341) 
REST 0.048, 0.002 = H(342,U[ISO]) 
REST 0.048, 0.002 = H(341,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(342) TO C ( 34) TO C(33) 
CONT H(342) TO C ( 34) TO C(35) 
CONT H(341) TO C ( 34) TO C(33) 
CONT H(341) TO C ( 34) TO C(35) 
ANGLE 109.54, 2.0 = 
CONT H(342) TO C ( 34) TO H(341) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 35) TO H(351) 
CONT C ( 35) TO H(352) 
REST 0.045, 0.002 = H(351,U[ISO]) 
REST 0.045, 0.002 = H(352,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(351) TO C ( 35) TO C(34) 
CONT H(351) TO C ( 35) TO C(36) 
CONT H(352) TO C ( 35) TO C(34) 
CONT H(352) TO C ( 35) TO C(36) 
ANGLE 109.54, 2.0 = 
CONT H(351) TO C ( 35) TO H(352) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 36) TO H(361) 
CONT C ( 36) TO H(362) 
REST 0.045, 0.002 = H(361,U[ISO]) 
REST 0.045, 0.002 = H(362,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(361) TO C ( 36) TO C(35) 
CONT H(361) TO C ( 36) TO C(31) 
CONT H(362) TO C ( 36) TO C(35) 
CONT H(362) TO C ( 36) TO C(31) 
ANGLE 109.54, 2.0 = 
CONT H(361) TO C ( 36) TO H(362) 
REM            1 H ON SP 3 
DIST 0.98, 0.02 = 
CONT C ( 41) TO H(411) 
REST 0.034, 0.002 = H(411,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(411) TO C ( 41) TO P(2) 
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 0.046, 0.002 = H(421,U[ISO]) 
REST 0.046, 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(432) 
CONT C ( 43) TO H(431) 
REST 0.053, 0.002 = H(432,U[ISO]) 
REST 0.053, 0.002 = H(431,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(432) TO C ( 43) TO C(42) 
CONT H(432) TO C ( 43) TO C(44) 
CONT H(431) TO C ( 43) TO C(42) 
CONT H(431) TO C ( 43) TO C(44) 
ANGLE 109.54, 2.0 = 
CONT H(432) TO C ( 43) TO H(431) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 44) TO H(441) 
CONT C ( 44) TO H(442) 
REST 0.051, 0.002 = H(441,U[ISO]) 
REST 0.051, 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 0.059, 0.002 = H(451,U[ISO]) 
REST 0.059, 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(462) 
CONT C ( 46) TO H(461) 
REST 0.055, 0.002 = H(462,U[ISO]) 
REST 0.055, 0.002 = H(461,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(462) TO C ( 46) TO C(45) 
CONT H(462) TO C ( 46) TO C(41) 
CONT H(461) TO C ( 46) TO C(45) 
CONT H(461) TO C ( 46) TO C(41) 
ANGLE 109.54, 2.0 = 
CONT H(462) TO C ( 46) TO H(461) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;