High-Nuclearity Metal-Cyanide Clusters: Synthesis, Magnetic Properties, and Inclusion Behavior of Open-Cage Species Incorporating [(tach)M(CN)3] (M = Cr, Fe, Co) Complexes
Jenny Y. Yang; Matthew P. Shores; Jennifer J. Sokol; Jeffrey R. Long; Inorganic Chemistry 42 (2003) 1403–1419; doi:10.1021/ic026065f

data_4313303
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 High-Nuclearity Metal-Cyanide Clusters: Synthesis, Magnetic Properties,
 and Inclusion Behavior of Open-Cage Species Incorporating [(tach)M(CN)3]
 (M = Cr, Fe, Co) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1403
_journal_page_last               1419
_journal_paper_doi               10.1021/ic026065f
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        synthetic
_chemical_formula_structural
;
 [(C6H15N3)8(H2O)6Cu6Co8(CN)24(C4H8O)]Br12-29(H2O)
;
_chemical_formula_sum            'C76 H198 Br12 Co8 Cu6 N48 O36'
_chemical_formula_weight         4172.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   19.2757(13)
_cell_length_b                   19.2757(13)
_cell_length_c                   37.008(3)
_cell_measurement_temperature    159(2)
_cell_volume                     11908.2(15)
_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      159(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  0.1005
_diffrn_reflns_av_sigmaI/netI    0.1146
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            16312
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    4.693
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.546864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             6264
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         3819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_obs          0.0578
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+196.4200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1740
_refine_ls_wR_factor_obs         0.1506
_reflns_number_observed          2702
_reflns_number_total             3819
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic026065f-2_s2_14.cif
_cod_data_source_block           14
_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^)+(0.0450P)^2^+196.4200P] 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^)+(0.0450P)^2^+196.4200P] 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        11908.1(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4313303
_diffrn_measurement_detector     'CCD area detector'