Giant Metal-Cyanide Coordination Clusters: Tetracapped Edge-Bridged Cubic Cr12Ni12(CN)48 and Double Face-Centered Cubic Cr14Ni13(CN)48 Species
Jennifer J. Sokol; Matthew P. Shores; Jeffrey R. Long; Inorganic Chemistry 41 (2002) 3052–3054; doi:10.1021/ic0255499

data_4318121
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 Giant Metal-Cyanide Coordination Clusters: Tetracapped Edge-Bridged Cubic
 Cr12Ni12(CN)48 and Double Face-Centered Cubic Cr14Ni13(CN)48 Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3052
_journal_page_last               3054
_journal_paper_doi               10.1021/ic0255499
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        synthetic
_chemical_formula_structural
;
 {[(C9H21N3)12Cr12Ni12(CN)48][K(C4H8O)4(H2O)2]}I12(KCN)-40(H2O)
;
_chemical_formula_sum            'C173 H368 Cr12 I12 K N85 Ni12 O46'
_chemical_formula_weight         7265.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      87
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.2490(15)
_cell_length_b                   24.2490(15)
_cell_length_c                   31.304(3)
_cell_measurement_temperature    154(2)
_cell_volume                     18407(2)
_computing_cell_refinement
;
  SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      154(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       'omega scans with profile analysis'
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17962
_diffrn_reflns_theta_max         16.51
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.010
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.815761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_meas      ?
_exptl_crystal_description       triangular_prism
_exptl_crystal_F_000             7296
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.136
_refine_ls_goodness_of_fit_obs   1.184
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2541
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.184
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_obs          0.1132
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1631P)^2^+545.6217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2988
_refine_ls_wR_factor_obs         0.2802
_reflns_number_observed          2073
_reflns_number_total             2541
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0255499_s2_2.cif
_cod_data_source_block           1
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
calc w=1/[\s^2^(Fo^2^)+(0.1631P)^2^+545.6217P] where
P=(Fo^2^+2Fc^2^)/3 ' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w=1/[\s^2^(Fo^2^)+(0.1631P)^2^+545.6217P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        18407.5(23)
_cod_database_code               4318121
_diffrn_measurement_detector     'CCD area detector'