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

data_7043026
_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         'C16 H24 B1 P2, As1 F6'
_chemical_formula_sum            'C16 H24 As B F6 P2'
_chemical_formula_weight         478.03
_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             14-02-10
_audit_creation_method           CRYSTALS_ver_14.23
_audit_update_record
;
2017-02-03 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3927(5)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   11.03020(10)
_cell_length_b                   16.4541(2)
_cell_length_c                   35.0725(5)
_cell_measurement_reflns_used    96362
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.55
_cell_volume                     6354.22(13)
_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 0.998
_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  0.070
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            77060
_diffrn_reflns_theta_full        27.477
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.562
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.804
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.80
_refine_diff_density_min         -1.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9629
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         14557
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.0008437
_refine_ls_shift/su_mean         0.0000261
_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: 
 19.8 28.6 13.9 3.40 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1606
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1606
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              45
_reflns_limit_l_min              0
_reflns_number_gt                10395
_reflns_number_total             14566
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.84
_oxford_diffrn_Wilson_scale      56.53
_oxford_refine_ls_r_factor_ref   0.0894
_oxford_refine_ls_scale          0.16026(7)
_oxford_reflns_number_all        14557
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'jas138 At 9:40 on 10/ 2'
_cod_data_source_file            c7dt01023k2.cif
_cod_data_source_block           jas138
_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        'C16 H24 As1 B1 F6 P2'
_cod_database_code               7043026
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
U(IJ) 0.0, 0.01 = F(21) TO F(22) 
U(IJ) 0.0, 0.01 = F(22) TO F(23) 
U(IJ) 0.0, 0.01 = F(23) TO F(24) 
U(IJ) 0.0, 0.01 = F(24) TO F(25) 
U(IJ) 0.0, 0.01 = F(25) TO F(26) 
U(IJ) 0.0, 0.01 = F(26) TO F(21) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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