A zwitterionic hydrocarbon-soluble borenium ion based on a β-diketiminate backbone
Abdalla, Joseph A. B.; Tirfoin, Rémi C.; Niu, Haoyu; Aldridge, Simon; Chem. Commun.  (2017) –; doi:10.1039/C7CC03121A

data_7120105
_publ_section_title
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 A zwitterionic hydrocarbon-soluble borenium ion based on a
 \b-diketiminate backbone
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03121A
_journal_year                    2017
_chemical_formula_moiety         'C59 H69 Al1 B1 Cl1 F15 K1 N2 O2'
_chemical_formula_sum            'C59 H69 Al B Cl F15 K N2 O2'
_chemical_formula_weight         1235.52
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-11-11
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2017-04-18 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                102.002(5)
_cell_angle_beta                 98.529(5)
_cell_angle_gamma                110.113(5)
_cell_formula_units_Z            2
_cell_length_a                   12.7841(7)
_cell_length_b                   13.6797(8)
_cell_length_c                   19.6984(11)
_cell_measurement_reflns_used    9430
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     3072.2(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32711
_diffrn_reflns_theta_full        73.258
_diffrn_reflns_theta_max         76.311
_diffrn_reflns_theta_min         3.583
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.062
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.98
_refine_diff_density_min         -0.96
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         12594
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.0005484
_refine_ls_shift/su_mean         0.0000308
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 8.56P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2051
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2050
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8954
_reflns_number_total             12645
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.28
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0967
_oxford_refine_ls_scale          5.00(9)
_oxford_reflns_number_all        12596
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title '132jart13 in P-1'
_cod_data_source_file            c7cc03121a2.cif
_cod_data_source_block           132JART13
_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      'P -1 '
_cod_original_formula_sum        'C59 H69 Al1 B1 Cl1 F15 K1 N2 O2'
_cod_database_code               7120105
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) H   (  93,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 223,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 263,X'S) H   ( 262,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) H   ( 272,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) H   ( 333,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 342,X'S) H   ( 343,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) H   ( 362,X'S) H   ( 363,X'S) 
RIDE C   (  37,X'S) H   ( 373,X'S) H   ( 372,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) H   ( 383,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) H   ( 733,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) H   ( 742,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) H   ( 772,X'S) H   ( 773,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  79,X'S) H   ( 793,X'S) H   ( 792,X'S) H   ( 791,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) H   ( 802,X'S) 
RIDE C   (  81,X'S) H   ( 813,X'S) H   ( 812,X'S) H   ( 811,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) H   ( 832,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) H   ( 842,X'S) 
RIDE C(85,X'S) H(854,X'S) H(855,X'S) H(856,X'S) H(851,X'S) H(852,X'S) H(853,X'S)
 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
REM 
REM ET2O DISORDER 
REM 
SAME  O(75)  C(78)  C(79) AND 
CONT  O(75)  C(76)  C(77) AND 
CONT  O(82)  C(83)  C(85) AND 
CONT  O(82)  C(84)  C(85) 
SIMU 0.01 O(75)  C(78)  C(79) AND 
CONT  O(75)  C(76)  C(77) AND 
CONT  O(82)  C(83)  C(85) AND 
CONT  O(82)  C(84)  C(85) 
DELU 0.01 O(75)  C(78)  C(79) AND 
CONT  O(75)  C(76)  C(77) AND 
CONT  O(82)  C(83)  C(85) AND 
CONT  O(82)  C(84)  C(85) 
END                                                                             
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