Dibismuthanes in catalysis: from synthesis and characterization to redox behavior towards oxidative cleavage of 1,2-diols.
Magre, Marc; Kuziola, Jennifer; Nöthling, Nils; Cornella, Josep; Organic & biomolecular chemistry 19 (2021) 4922–4929; doi:10.1039/d1ob00367d

data_7158064
_publ_section_title
;
 Dibismuthanes in catalysis: from synthesis and characterization to redox
 behavior towards oxidative cleavage of 1,2-diols.
;
_journal_issue                   22
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4922
_journal_page_last               4929
_journal_paper_doi               10.1039/d1ob00367d
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C38 H30 Bi2 O'
_chemical_formula_sum            'C38 H30 Bi2 O'
_chemical_formula_weight         920.58
_chemical_name_systematic
;
4,6-bis(diphenylbismuthanyl)-10,11-dihydrodibenzo[b,f]oxepine
;
_chemical_properties_physical    none
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                KUJ-KA-131-01
_audit_creation_date             2020-08-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-02-19 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                83.462(6)
_cell_angle_beta                 88.592(9)
_cell_angle_gamma                79.178(12)
_cell_formula_units_Z            2
_cell_length_a                   10.6951(17)
_cell_length_b                   10.8286(12)
_cell_length_c                   13.7009(8)
_cell_measurement_reflns_used    49119
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0996
_cell_measurement_theta_min      2.771
_cell_volume                     1548.4(3)
_computing_cell_refinement       'EVALCCD V. 1.6, 2008'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'EVALCCD V. 1.6, 2008'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2014)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios focusing multilayer optics'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47337
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.080
_diffrn_reflns_theta_min         2.768
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.378
_exptl_absorpt_correction_T_max  0.68309
_exptl_absorpt_correction_T_min  0.47746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent:  dichloromethane, hexane'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         11728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+1.7413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8776
_reflns_number_total             11728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ob00367d2.cif
_cod_data_source_block           13364sadabs
_cod_depositor_comments
'Adding full bibliography for 7158061--7158068.cif.'
_cod_database_code               7158064
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C12(H12), C34(H34), C28(H28), C13(H13), C26(H26), C2(H2), C22(H22),
 C29(H29), C31(H31), C20(H20), C19(H19), C32(H32), C16(H16), C38(H38), C35(H35),
  C14(H14), C25(H25), C36(H36), C17(H17), C23(H23), C37(H37), C18(H18), C3(H3),
 C24(H24), C4(H4)
;
_shelx_res_checksum              71983
_shelx_hkl_checksum              33199
_olex2_submission_special_instructions 'No special instructions were received'