Redetermination of ammonium bisoxalatobismuthate(III) <i>x</i>-hydrate from single-crystal data
Yang, Jun-Ying; Fu, Yun-Long; Chu, Jia; Ng, Seik Weng; Acta Crystallographica Section E 62 (2006) m2310–m2312; doi:10.1107/S1600536806033186

data_2210409
_publ_section_title
;
 Redetermination of ammonium bisoxalatobismuthate(III) <i>x</i>-hydrate
 from single-crystal data
;
_journal_coeditor_code           WM2042
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2310
_journal_page_last               m2312
_journal_paper_doi               10.1107/S1600536806033186
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'N H4 [Bi (C2 O4)2], 3.72H2 O'
_chemical_formula_moiety         'N H4 + C4 Bi1 O8 -, 3.72H2 O'
_chemical_formula_sum            'C4 H11.44 Bi N O11.72'
_chemical_formula_weight         470.38
_chemical_name_systematic
;
poly[ammonium di-\m~2~-oxalato-bismuthate(III) 3.72-hydrate]
;
_space_group_IT_number           141
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   isomor
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6740(10)
_cell_length_b                   11.6740(10)
_cell_length_c                   9.2545(8)
_cell_measurement_reflns_used    2126
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.6
_cell_volume                     1261.22(19)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    '<i>X-SEED</i> (Barbour, 2001)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'atomic coordinates taken from published structure'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.016
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3231
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.8
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.036
_exptl_absorpt_correction_T_max  0.199
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             878
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.13
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         401
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.13
_refine_ls_R_factor_all          0.025
_refine_ls_R_factor_gt           0.023
_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^)+(0.0476P)^2^+3.0591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.067
_refine_ls_wR_factor_ref         0.068
_reflns_number_gt                365
_reflns_number_total             401
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2042.cif
_cod_data_source_block           I
_cod_original_cell_volume        1261.2(2)
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               2210409
_cod_database_fobs_code          2210409