Coordination of a stibine oxide to a Lewis acidic stiborane at the upper rim of the biphenylene backbone.
Chen, Chang-Hong; Gabbaï, François P; Dalton transactions (Cambridge, England : 2003) 47 (2018) 12075–12078; doi:10.1039/c8dt02872a

data_7047209
_publ_section_title
;
 Coordination of a stibine oxide to a Lewis acidic stiborane at the upper
 rim of the biphenylene backbone.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12075
_journal_page_last               12078
_journal_paper_doi               10.1039/c8dt02872a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C36 H26 Sb2'
_chemical_formula_sum            'C36 H26 Sb2'
_chemical_formula_weight         702.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-07-13 deposited with the CCDC.
2018-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.512(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.205(3)
_cell_length_b                   17.811(9)
_cell_length_c                   12.643(6)
_cell_measurement_reflns_used    4404
_cell_measurement_temperature    110
_cell_measurement_theta_max      25.857
_cell_measurement_theta_min      2.287
_cell_volume                     1388.3(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0630
_diffrn_reflns_av_unetI/netI     0.0921
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13087
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.782
_diffrn_reflns_theta_min         1.621
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1077 before and 0.0813 after correction. The Ratio of minimum to maximum transmission is 0.8047. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.705
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 2192 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5877
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0321P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0986
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                5239
_reflns_number_total             5877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02872a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7047209--7047210.cif.'
_cod_original_cell_volume        1388.2(12)
_cod_database_code               7047209
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C16(H16), C22(H22), C4(H4), C23(H23), C3(H3), C24(H24),
 C14(H14), C21(H21), C18(H18), C2(H2), C15(H15), C11(H11), C20(H20), C17(H17),
 C26(H26), C32(H32), C27(H27), C30(H30), C28(H28), C29(H29), C34(H34), C33(H33),
  C36(H36), C35(H35)
;
_shelx_res_checksum              48175
_olex2_submission_special_instructions 'No special instructions were received'