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_4069470
_publ_section_title
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 Synthesis, Ethanolysis, and Hydrolysis of Bismuth(III)ortho-Nitrobenzoate
 Complexes en Route to a Pearl Necklace-like Polymer of Bi10Oxo-Clusters
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_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
'C208 H148 Bi20 N28 O134, C210 H154 Bi20 N28 O135, 8(C2 H6 O), 4(H2 O)'
_chemical_formula_sum            'C434 H356 Bi40 N56 O281'
_chemical_formula_weight         19210.95
_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                89.761(2)
_cell_angle_beta                 89.313(2)
_cell_angle_gamma                87.692(2)
_cell_formula_units_Z            1
_cell_length_a                   17.6559(6)
_cell_length_b                   21.4220(7)
_cell_length_c                   35.9678(11)
_cell_measurement_reflns_used    155369
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      0
_cell_volume                     13591.8(8)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0878
_diffrn_reflns_av_sigmaI/netI    0.1572
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            95045
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.004
_exptl_absorpt_correction_T_max  0.4227
_exptl_absorpt_correction_T_min  0.3288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             8920
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.776
_refine_diff_density_min         -2.287
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1770
_refine_ls_number_reflns         47427
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1576
_reflns_number_gt                26857
_reflns_number_total             47427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9002158_si_002.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_database_code               4069470