An Acid-Free Anionic Oxoborane Isoelectronic with Carbonyl: Facile Access and Transfer of a Terminal B═O Double Bond.
Loh, Ying Kai; Porteous, Kieran; Fuentes, M Ángeles; Do, Dinh Cao Huan; Hicks, Jamie; Aldridge, Simon; Journal of the American Chemical Society 141 (2019) 8073–8077; doi:10.1021/jacs.9b03600

data_4127231
_publ_section_title
;
 An Acid-Free Anionic Oxoborane Isoelectronic with Carbonyl: Facile Access
 and Transfer of a Terminal B&#x2550;O Double Bond.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8073
_journal_page_last               8077
_journal_paper_doi               10.1021/jacs.9b03600
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C26 H36 B N2 S, C18 H36 K N2 O6, 4(C6 H6)'
_chemical_formula_sum            'C68 H96 B K N4 O6 S'
_chemical_formula_weight         1147.45
_chemical_melting_point          ?
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                80.367(2)
_cell_angle_beta                 86.833(2)
_cell_angle_gamma                86.675(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0099(3)
_cell_length_b                   15.9376(4)
_cell_length_c                   16.4118(4)
_cell_measurement_reflns_used    23405
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.0920
_cell_measurement_theta_min      3.5350
_cell_volume                     3345.71(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXLE (HUbschle, 2017)'
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5035
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47664
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.225
_diffrn_reflns_theta_min         3.588
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         13834
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.6012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12377
_reflns_number_total             13834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03600_si_002.cif
_cod_data_source_block           197ykmaf18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4127230--4127234.cif.
;
_cod_database_code               4127231
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.724
_shelx_estimated_absorpt_t_max   0.770
_shelx_res_checksum              85150
_shelx_hkl_checksum              58799