Hydrolysis Studies on Bismuth Nitrate: Synthesis and Crystallization of Four Novel Polynuclear Basic Bismuth Nitrates
L. Miersch; T. Rüffer; M. Schlesinger; H. Lang; M. Mehring; Inorganic Chemistry 51 (2012) 9376–9384; doi:10.1021/ic301148p

data_4330183
_publ_section_title
;
 Hydrolysis Studies on Bismuth Nitrate: Synthesis and Crystallization of
 Four Novel Polynuclear Basic Bismuth Nitrates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9376
_journal_page_last               9384
_journal_paper_doi               10.1021/ic301148p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C53.5 H160.5 Bi38 N24 O144 S27'
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_chemical_name_systematic
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 ?
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_atom_sites_solution_primary     direct
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_cell_angle_gamma                60.228(5)
_cell_formula_units_Z            2
_cell_length_a                   20.3804(10)
_cell_length_b                   20.3871(9)
_cell_length_c                   34.9715(15)
_cell_measurement_reflns_used    45328
_cell_measurement_temperature    110
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_computing_cell_refinement
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
(compiled Jun 12 2006,17:01:16)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
(compiled Jun 12 2006,17:01:16)
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
(compiled Jun 12 2006,17:01:16)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
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_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       '\w scans'
_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  0.0661
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_diffrn_reflns_limit_h_max       24
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_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            95002
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  5
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_exptl_absorpt_coefficient_mu    28.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49309
_exptl_absorpt_correction_type   multi-scan
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;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.5 (release 12-06-2006 CrysAlis171 .NET)
(compiled Jun 12 2006,17:01:16)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.385
_exptl_crystal_description       block
_exptl_crystal_F_000             10775
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_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.872
_refine_diff_density_min         -5.886
_refine_diff_density_rms         0.477
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     2602
_refine_ls_number_reflns         46210
_refine_ls_number_restraints     1111
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1883
_reflns_number_gt                28606
_reflns_number_total             46210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301148p_si_001_3.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        12021.7(9)
_cod_original_formula_sum        'C53.50 H160.50 Bi38 N24 O144 S27'
_cod_database_code               4330183