Synthesis, Ethanolysis, and Hydrolysis of Bismuth(III)ortho-Nitrobenzoate Complexes en Route to a Pearl Necklace-like Polymer of Bi10Oxo-Clusters
Andrews, Philip C.; Deacon, Glen B.; Junk, Peter C.; Kumar, Ish; MacLellan, Jonathan G.; Organometallics 28 (2009) 3999–; doi:10.1021/om9002158

data_4069467
_publ_section_title
;
 Synthesis, Ethanolysis, and Hydrolysis of Bismuth(III)ortho-Nitrobenzoate
 Complexes en Route to a Pearl Necklace-like Polymer of Bi10Oxo-Clusters
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3999
_journal_paper_doi               10.1021/om9002158
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C21 H14 Bi N3 O13'
_chemical_formula_sum            'C21 H14 Bi N3 O13'
_chemical_formula_weight         725.33
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.2150(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4029(3)
_cell_length_b                   6.97800(10)
_cell_length_c                   26.3531(4)
_cell_measurement_reflns_used    26212
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.63
_cell_volume                     2244.64(7)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker Axs 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker Axs 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker Axs 2005)'
_computing_molecular_graphics    'X-seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 Apex KAPPA CCD'
_diffrn_measurement_method       '0.5 deg frames in phi and omega'
_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  0.0756
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17968
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.936
_exptl_absorpt_correction_T_max  0.5302
_exptl_absorpt_correction_T_min  0.4179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.970
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5155
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0323P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                3683
_reflns_number_total             5155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9002158_si_002.cif
_cod_data_source_block           Compound1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4069467