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

data_7043027
_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 B2 Br4 P2'
_chemical_formula_sum            'C26 H50 B2 Br4 P2'
_chemical_formula_weight         765.87
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2013-06-07 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.666(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4285(7)
_cell_length_b                   8.5936(3)
_cell_length_c                   20.9657(8)
_cell_measurement_reflns_used    14946
_cell_measurement_temperature    273
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.55
_cell_volume                     3309.3(2)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      273
_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  0.073
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22553
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.617
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.976
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.58
_refine_diff_density_min         -1.03
_refine_ls_extinction_coef       110(30)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9337
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2903
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.0006748
_refine_ls_shift/su_mean         0.0000337
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ +24.01P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1817
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1817
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                2052
_reflns_number_total             2903
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.53
_oxford_diffrn_Wilson_scale      79.73
_oxford_refine_ls_r_factor_ref   0.0899
_oxford_refine_ls_scale          0.12927(18)
_oxford_reflns_number_all        2903
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c7dt01023k2.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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      'C 2/c '
_cod_database_code               7043027
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE B   (   1,X'S) H   (   1,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) H   ( 132,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
U(IJ) 0.0, 0.01 = C(11) TO C(12) 
U(IJ) 0.0, 0.01 = C(12) TO C(13) 
U(IJ) 0.0, 0.01 = C(13) TO C(14) 
U(IJ) 0.0, 0.01 = C(14) TO C(15) 
U(IJ) 0.0, 0.01 = C(15) TO C(16) 
U(IJ) 0.0, 0.01 = C(16) TO C(11) 
REM 
DIST 0.0, 0.01 = MEAN C(11) TO C(12), C(12) TO C(13) 
DIST 0.0, 0.01 = MEAN C(12) TO C(13), C(13) TO C(14) 
DIST 0.0, 0.01 = MEAN C(13) TO C(14), C(14) TO C(15) 
DIST 0.0, 0.01 = MEAN C(14) TO C(15), C(15) TO C(16) 
DIST 0.0, 0.01 = MEAN C(15) TO C(16), C(16) TO C(11) 
DIST 0.0, 0.01 = MEAN C(16) TO C(11), C(11) TO C(12) 
REM 
ANGLE 0.0, 1. = MEAN C(11) TO C(12) TO C(13), C(12) TO C(13) TO C(14) 
ANGLE 0.0, 1. = MEAN C(12) TO C(13) TO C(14), C(13) TO C(14) TO C(15) 
ANGLE 0.0, 1. = MEAN C(13) TO C(14) TO C(15), C(14) TO C(15) TO C(16) 
ANGLE 0.0, 1. = MEAN C(14) TO C(15) TO C(16), C(15) TO C(16) TO C(11) 
ANGLE 0.0, 1. = MEAN C(15) TO C(16) TO C(11), C(16) TO C(11) TO C(12) 
ANGLE 0.0, 1. = MEAN C(16) TO C(11) TO C(12), C(11) TO C(12) TO C(13) 
REM 
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(11) 
CONT C ( 1) TO H(12) 
REST 0.054, 0.002 = H(11,U[ISO]) 
REST 0.054, 0.002 = H(12,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(11) TO C ( 1) TO C(1,-1,2,0,0,1) 
CONT H(11) TO C ( 1) TO P(1) 
CONT H(12) TO C ( 1) TO C(1,-1,2,0,0,1) 
CONT H(12) TO C ( 1) TO P(1) 
ANGLE 109.54, 2.0 = 
CONT H(11) TO C ( 1) TO H(12) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 12) TO H(121) 
CONT C ( 12) TO H(122) 
REST 0.128, 0.002 = H(121,U[ISO]) 
REST 0.128, 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 0.102, 0.002 = H(131,U[ISO]) 
REST 0.102, 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            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 14) TO H(141) 
REST 0.138, 0.002 = H(141,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(141) TO C ( 14) TO C(13) 
CONT H(141) TO C ( 14) TO C(15) 
PLANAR C ( 14) C(13) C(15) H(141) 
REM            1 H ON SP 2 
DIST 0.93, 0.02 = 
CONT C ( 15) TO H(151) 
REST 0.139, 0.002 = H(151,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) 
PLANAR C ( 15) C(14) C(16) H(151) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 16) TO H(161) 
CONT C ( 16) TO H(162) 
REST 0.084, 0.002 = H(161,U[ISO]) 
REST 0.084, 0.002 = H(162,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(161) TO C ( 16) TO C(15) 
CONT H(161) TO C ( 16) TO C(11) 
CONT H(162) TO C ( 16) TO C(15) 
CONT H(162) TO C ( 16) TO C(11) 
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 0.056, 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 0.071, 0.002 = H(221,U[ISO]) 
REST 0.071, 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(231) 
CONT C ( 23) TO H(232) 
REST 0.079, 0.002 = H(231,U[ISO]) 
REST 0.079, 0.002 = H(232,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) 
CONT H(232) TO C ( 23) TO C(22) 
CONT H(232) TO C ( 23) TO C(24) 
ANGLE 109.54, 2.0 = 
CONT H(231) TO C ( 23) TO H(232) 
REM            2 H ON SP 3 
DIST 0.97, 0.02 = 
CONT C ( 24) TO H(241) 
CONT C ( 24) TO H(242) 
REST 0.092, 0.002 = H(241,U[ISO]) 
REST 0.092, 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 0.109, 0.002 = H(251,U[ISO]) 
REST 0.109, 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 0.086, 0.002 = H(261,U[ISO]) 
REST 0.086, 0.002 = H(262,U[ISO]) 
ANGLE 0.0, 2.0 = MEAN 
CONT H(261) TO C ( 26) TO C(21) 
CONT H(261) TO C ( 26) TO C(25) 
CONT H(262) TO C ( 26) TO C(21) 
CONT H(262) TO C ( 26) TO C(25) 
ANGLE 109.54, 2.0 = 
CONT H(261) TO C ( 26) TO H(262) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;