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_4318120
_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
;
 {Ni[(C9H21N3)7Cr7Ni6(CN)24]2}I20-70H2O
;
_chemical_formula_sum            'C174 H434 Cr14 I20 N90 Ni13 O70'
_chemical_formula_weight         8937.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            4
_cell_length_a                   23.2283(9)
_cell_length_b                   34.683(2)
_cell_length_c                   46.900(2)
_cell_measurement_temperature    160(2)
_cell_volume                     37784(3)
_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      160(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  0.1024
_diffrn_reflns_av_sigmaI/netI    0.1022
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            24393
_diffrn_reflns_theta_max         14.74
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.482928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             17712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.217
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         7186
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.208
_refine_ls_R_factor_all          0.2308
_refine_ls_R_factor_obs          0.1703
_refine_ls_shift/esd_max         -1.745
_refine_ls_shift/esd_mean        0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2721P)^2^+2243.7224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.4801
_refine_ls_wR_factor_obs         0.4228
_reflns_number_observed          4313
_reflns_number_total             7187
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0255499_s2_1.cif
_cod_data_source_block           2
_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^)+(0.2721P)^2^+2243.7224P] 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^)+(0.2721P)^2^+2243.7224P] 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        37783.5(26)
_cod_database_code               4318120
_diffrn_measurement_detector     'CCD area detector'