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

data_7043010
_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         'C41 H41 B1 P3, As1 F6, H2 O1'
_chemical_formula_sum            'C41 H43 As B F6 O P3'
_chemical_formula_weight         844.43
_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     other
_audit_creation_date             13-08-24
_audit_creation_method           CRYSTALS_ver_14.23
_audit_update_record
;
2015-04-08 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.315(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2239(6)
_cell_length_b                   21.5110(9)
_cell_length_c                   14.3499(4)
_cell_measurement_reflns_used    45439
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     4016.0(3)
_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      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.165
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            55977
_diffrn_reflns_theta_full        26.068
_diffrn_reflns_theta_max         26.068
_diffrn_reflns_theta_min         2.704
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/acetone/pentane'
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.36
_refine_diff_density_min         -1.82
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9314
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7920
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.0005213
_refine_ls_shift/su_mean         0.0000387
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 6.29P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1932
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1932
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3988
_reflns_number_total             7922
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.10
_oxford_diffrn_Wilson_scale      130.14
_oxford_refine_ls_r_factor_ref   0.1601
_oxford_refine_ls_scale          0.11012(6)
_oxford_reflns_number_all        7920
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'jas127 At 14:37 on 24/ 8'
_cod_data_source_file            c7dt01023k2.cif
_cod_data_source_block           jas127
_cod_depositor_comments
;
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      'P 21/n '
_cod_original_formula_sum        'C41 H43 As1 B1 F6 O1 P3'
_cod_database_code               7043010
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
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   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) H   (  53,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   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.01 = C(41) TO C(42) 
U(IJ) 0.0, 0.01 = C(42) TO C(43) 
U(IJ) 0.0, 0.01 = C(43) TO C(44) 
U(IJ) 0.0, 0.01 = C(44) TO C(45) 
U(IJ) 0.0, 0.01 = C(45) TO C(46) 
U(IJ) 0.0, 0.01 = C(46) TO C(41) 
REM DIST 1.0, 0.01 = O(101) TO H(1011) 
REM DIST 0.88, 0.01 = O(101) TO H(1012) 
REM ANGLE 109.0, 0.05 = H(1011) TO O(101) TO H(1012) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;