Mixed-Valent Dodecanuclear Vanadium Cluster Encapsulating Chloride Anions and Its Reaction To Form a "Bowl"-Shaped Cluster
Sanjit Konar; Abraham Clearfield; Inorganic Chemistry 47 (2008) 3492–3494; doi:10.1021/ic800013f

data_4304911
_publ_contact_author
; 
'Abraham Clearfield'
;
_publ_contact_author_email       clearfield@mail.chem.tamu.edu
_publ_contact_author_phone       '+1 979 997 9299'
_publ_section_title
;
Mixed-Valent Dodecanuclear Vanadium Cluster Encapsulating Chloride Anions
and Its Reaction To Form a "Bowl"-Shaped Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3492
_journal_page_last               3494
_journal_paper_doi               10.1021/ic800013f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C124 H141 Cl2 N6 O63 P8 V12'
_chemical_formula_weight         3653.37
_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                86.430(11)
_cell_angle_beta                 81.083(10)
_cell_angle_gamma                78.355(11)
_cell_formula_units_Z            2
_cell_length_a                   17.528(11)
_cell_length_b                   19.255(12)
_cell_length_c                   25.444(15)
_cell_measurement_temperature    110(2)
_cell_volume                     8305(9)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.1180
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66876
_diffrn_reflns_theta_full        23.39
_diffrn_reflns_theta_max         23.39
_diffrn_reflns_theta_min         0.81
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2.10'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             3722
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.051
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1966
_refine_ls_number_reflns         23975
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.2076
_refine_ls_R_factor_gt           0.1353
_refine_ls_shift/su_max          2.263
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1752P)^2^+189.8590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3395
_refine_ls_wR_factor_ref         0.4024
_reflns_number_gt                13525
_reflns_number_total             23975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800013f-file001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4304911