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

data_7043016
_publ_section_title
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 Synthetic and Structural Studies of Phosphine Coordinated Boronium Salts
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_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 H26 B1 P2, Br1, C0.89 H1.79, Cl1.79'
_chemical_formula_sum            'C26.89 H27.79 B Br Cl1.79 P2'
_chemical_formula_weight         566.96
_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.
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_cell_angle_alpha                90
_cell_angle_beta                 101.3055(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8454(2)
_cell_length_b                   15.8917(3)
_cell_length_c                   14.0831(3)
_cell_measurement_reflns_used    59767
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     2819.07(9)
_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 0.997
_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  0.040
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56899
_diffrn_reflns_theta_full        27.535
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         2.714
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  0.718
_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    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1157.941
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.91
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6465
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.0020679
_refine_ls_shift/su_mean         0.0000915
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 3.53P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1540
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1540
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5240
_reflns_number_total             6480
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.92
_oxford_diffrn_Wilson_scale      3.83
_oxford_refine_ls_r_factor_ref   0.0649
_oxford_refine_ls_scale          0.6168(16)
_oxford_reflns_number_all        6465
_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:

'_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_original_formula_sum        'C26.89 H27.79 B1 Br1 Cl1.79 P2'
_cod_database_code               7043016
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT CL(10, OCC) CL(11, OCC) 
EQUIV CL(10, OCC) CL(11, OCC) 
WEIGHT -1 CL(10, OCC) 
RIDE B   (   1,X'S) H   (   1,X'S) H   (   2,X'S) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,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   (  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   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,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   (  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   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
CONT H   ( 511,X'S) H   ( 512,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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U(IJ) 0.0, 0.02 = CL(10) TO CL(11) 
DIST 0.0, 0.05 = MEAN C(50) TO CL(10), C(50) TO CL(11) 
ANGLE 0.0, 3. = MEAN CL(10) TO C(50) TO CL(2), CL(11) TO C(50) TO CL(2) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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