Synthesis and structural studies of the simplest bismuth(III) oxo-salicylate complex: [Bi4(mu3-O)2(HO-2-C6H4CO2)8].2Solv (Solv = MeCN or MeNO2)
Tyler D. Boyd; Ish Kumar; Eric E. Wagner; Kenton H. Whitmire; Chem.Commun. 50 (2014) 3556–; doi:10.1039/C4CC00056K

data_7112127
_publ_section_title
;
 Synthesis and structural studies of the simplest bismuth(III)
 oxo-salicylate complex: [Bi4(mu3-O)2(HO-2-C6H4CO2)8].2Solv (Solv = MeCN
 or MeNO2)
;
_journal_name_full               Chem.Commun.
_journal_page_first              3556
_journal_paper_doi               10.1039/C4CC00056K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C56 H40 Bi4 O26, 2(C2 H3 N)'
_chemical_formula_sum            'C60 H46 Bi4 N2 O26'
_chemical_formula_weight         2046.91
_chemical_name_systematic
;
tetrakis(salicylato)dioxotetrabismuth acetonitrile solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                69.9520(10)
_cell_angle_beta                 68.4760(10)
_cell_angle_gamma                77.0260(10)
_cell_formula_units_Z            1
_cell_length_a                   11.0416(9)
_cell_length_b                   11.4113(10)
_cell_length_c                   14.0227(12)
_cell_measurement_reflns_used    7279
_cell_measurement_temperature    298(2)
_cell_volume                     1534.2(2)
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  BRUKERSMART1000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19036
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_min         1.912
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    11.524
_exptl_absorpt_correction_T_max  0.056
_exptl_absorpt_correction_T_min  0.044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 5.1,1997'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.00434(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         7278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5930
_reflns_number_total             7278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00056k.cif
_cod_data_source_block           abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_database_code               7112127
_shelxl_version_number           2013-2
_shelx_res_checksum              96029