Carbon Monoxide Insertion at a Heavy p-Block Element: Unprecedented Formation of a Cationic Bismuth Carbamoyl
Ramler, Jacqueline; Poater, Jordi; Hrisch, Florian; Ritschel, Benedikt; Fischer, Ingo; Bickelhaupt, F. Matthias; Lichtenberg, Crispin; Chemical Science  (2019) –; doi:10.1039/C9SC00278B

data_1550681
_publ_section_title
;
 Carbon Monoxide Insertion at a Heavy p-Block Element: Unprecedented
 Formation of a Cationic Bismuth Carbamoyl
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00278B
_journal_year                    2019
_chemical_formula_moiety         'C24 H19 Bi F3 N3 O4 S'
_chemical_formula_sum            'C24 H19 Bi F3 N3 O4 S'
_chemical_formula_weight         711.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_audit_update_record
;
2019-01-17 deposited with the CCDC.    2019-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.4741(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1161(5)
_cell_length_b                   9.3373(3)
_cell_length_c                   18.4406(7)
_cell_measurement_reflns_used    7779
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.61
_cell_volume                     2438.36(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.756
_diffrn_reflns_theta_min         2.358
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.376
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6586
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0656 before and 0.0247 after correction.
The Ratio of minimum to maximum transmission is 0.8836.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_description       needle
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.640
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4112
_reflns_number_total             5190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00278b2.cif
_cod_data_source_block           Compound_2
_cod_database_code               1550681
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.436
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C23(H23), C8(H8), C9(H9), C5(H5), C14(H14), C11(H11), C12(H12),
 C18(H18), C4(H4), C6(H6), C16(H16), C15(H15), C19(H19), C10(H10), C20(H20),
 C17(H17), C21(H21), C22(H22)
;
_shelx_res_checksum              61366
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'