Isolation of Tetranuclear Organoantimony Oxo Clusters and Hexa-decanuclear Polyoxostibonates
Jami, Ananda Kumar; Prabhu, M. Santhana Raj; Baskar, Viswanathan; Organometallics 29 (2010) 1137–; doi:10.1021/om900942q

data_4083379
_publ_section_title
;
 Isolation of Tetranuclear Organoantimony Oxo Clusters and
 Hexa-decanuclear Polyoxostibonates
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1137
_journal_paper_doi               10.1021/om900942q
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C87 H65 Br4 Cl9 N8 O11 Sb4'
_chemical_formula_sum            'C87 H65 Br4 Cl9 N8 O11 Sb4'
_chemical_formula_weight         2524.16
_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                74.305(2)
_cell_angle_beta                 83.621(2)
_cell_angle_gamma                66.700(2)
_cell_formula_units_Z            2
_cell_length_a                   15.639(2)
_cell_length_b                   17.062(3)
_cell_length_c                   19.793(3)
_cell_measurement_reflns_used    6880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.34
_cell_volume                     4669.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39052
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    3.175
_exptl_absorpt_correction_T_max  0.5988
_exptl_absorpt_correction_T_min  0.4115
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   brukersadbas
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.844
_refine_diff_density_min         -1.546
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         18203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          6.108
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+9.7361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                14010
_reflns_number_total             18203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900942q_si_002.cif
_cod_data_source_block           COMPOUND_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4669.8(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4083379