Novel Sterically Congested Monoorganobismuth(III) Compounds: Synthesis, Structure, and Bismuth−Arene π Interaction in ArBiXY (X, Y = Br, I, OH, 2,6-Mes2-4-t-Bu-C6H2PHO2)
Breunig, Hans J.; Haddad, Nawja; Lork, Enno; Mehring, Michael; Mügge, Clemens; Nolde, Christof; Raţ, Ciprian I.; Schürmann, Markus; Organometallics 28 (2009) 1202–; doi:10.1021/om800934c

data_4068549
_publ_section_title
;
 Novel Sterically Congested Monoorganobismuth(III) Compounds: Synthesis,
 Structure, and Bismuth&#x2212;Arene \p Interaction in ArBiXY (X, Y = Br,
 I, OH, 2,6-Mes2-4-t-Bu-C6H2PHO2)
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1202
_journal_paper_doi               10.1021/om800934c
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C28 H33 Bi Br1.12 Cl0.88, C1 H2 Cl2'
_chemical_formula_sum            'C29 H35 Bi Br1.12 Cl2.88'
_chemical_formula_weight         784.15
_chemical_melting_point          479.5(15)
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.120(2)
_cell_angle_beta                 91.579(2)
_cell_angle_gamma                104.401(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9213(3)
_cell_length_b                   13.0022(6)
_cell_length_c                   14.2868(6)
_cell_measurement_reflns_used    13792
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.27
_cell_volume                     1524.91(11)
_computing_cell_refinement
;
DENZO & SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO & SCALEPACK
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
 3 sets at different \k-angles and 152 frames via \w-rotation 
(\D/\w=2\%) at two times 90s per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13792
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    7.516
_exptl_absorpt_correction_T_max  0.705
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6824
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                5014
_reflns_number_total             6824
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800934c_si_002.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '478-481k' was changed to '479.5(15)'
- the average value was taken and precision was
estimated.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26 (7
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.2 from 2011-04-26 (23 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068549