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

data_7043009
_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         'C34 H30 B1 Fe1 P2, Br4 Fe1'
_chemical_formula_sum            'C34 H30 B Br4 Fe2 P2'
_chemical_formula_weight         942.68
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_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             15-02-08
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2015-04-08 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1146(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.51940(10)
_cell_length_b                   15.98130(10)
_cell_length_c                   23.62910(10)
_cell_measurement_reflns_used    38517
_cell_measurement_temperature    150
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     3589.44(5)
_computing_cell_refinement       'CrysAlis PRO, (Agilent Technologies, 2013)'
_computing_data_collection       'SuperNova, (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlis PRO, (Agilent Technologies, 2013)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_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      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            70155
_diffrn_reflns_theta_full        72.409
_diffrn_reflns_theta_max         72.409
_diffrn_reflns_theta_min         3.340
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.713
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1844
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/pentane'
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.066
_platon_squeeze_details
;
;
_refine_diff_density_max         0.91
_refine_diff_density_min         -1.08
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9969
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7091
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.0010865
_refine_ls_shift/su_mean         0.0000273
_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: 
 0.242E+04 0.409E+04 0.265E+04 0.124E+04 375. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0869
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0869
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              -16
_reflns_limit_l_max              29
_reflns_limit_l_min              -29
_reflns_number_gt                6930
_reflns_number_total             7092
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0327
_oxford_refine_ls_scale          2.496(12)
_oxford_reflns_number_all        7091
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title
'C:\Users\Jas\Desktop\jas167(JSW4 At 9:41 on '
_cod_data_source_file            c7dt01023k2.cif
_cod_data_source_block           jas167(JSW418)(2)
_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        'C34 H30 B1 Br4 Fe2 P2'
_cod_database_code               7043009
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
REM CONT O(1, OCC) F(100, OCC) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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