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_4304912
_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            'C117 H75 Cl5 N6 O52 P6 V12'
_chemical_formula_weight         3371.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.8442(16)
_cell_length_b                   16.8442(16)
_cell_length_c                   34.778(7)
_cell_measurement_temperature    110(2)
_cell_volume                     8545(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            69116
_diffrn_reflns_theta_full        23.38
_diffrn_reflns_theta_max         23.38
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2.10'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3372
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.707
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.293
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_coef       0.0058(6)
_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   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          1.089
_refine_ls_shift/su_mean         0.142
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1368P)^2^+8.2902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1976
_reflns_number_gt                3977
_reflns_number_total             4250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800013f-file003.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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_original_cell_volume        8546(2)
_cod_database_code               4304912