Hybrid Cluster-Cages Formed via Cyanometalate Condensation: Cs@Co4Ru6S2(CN)12, Co4Ru9S6(CN)9, and Rh4Ru9S6(CN)9 Frameworks
Matthew L. Kuhlman; Thomas B. Rauchfuss; Inorganic Chemistry 43 (2004) 430–435; doi:10.1021/ic034745s

data_4310402
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Hybrid Cluster-Cages Formed via Cyanometalate Condensation:
 Cs@Co4Ru6S2(CN)12, Co4Ru9S6(CN)9, and Rh4Ru9S6(CN)9 Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              430
_journal_page_last               435
_journal_paper_doi               10.1021/ic034745s
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
; 
C82 H93 Co4 Cs N12 Ru6 S2, C82 H93 Co4 Cs N12 Ru6 S2, 4(F6 P), 
10(C2 H3 N) 
;
_chemical_formula_sum            'C92 H108 Co4 Cs F12 N17 P2 Ru6 S2'
_chemical_formula_weight         2781.06
_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
_audit_update_record
; 
2003-06-13    text and data added, mlk 
;
_cell_angle_alpha                111.742(6)
_cell_angle_beta                 91.535(7)
_cell_angle_gamma                93.373(6)
_cell_formula_units_Z            4
_cell_length_a                   15.586(4)
_cell_length_b                   26.955(8)
_cell_length_c                   28.378(8)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      16.3
_cell_measurement_theta_min      2.3
_cell_volume                     11040(5)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  p96paps
_diffrn_reflns_av_R_equivalents  0.1554
_diffrn_reflns_av_sigmaI/netI    0.3286
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26627
_diffrn_reflns_theta_full        17.25
_diffrn_reflns_theta_max         17.25
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        7.2
_diffrn_standards_interval_time  562
_diffrn_standards_number         85
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.7666
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platy
_exptl_crystal_F_000             5504
_exptl_crystal_id                p96paps
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (??) scattering planes 
roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         13345
_refine_ls_number_restraints     894
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.2138
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                4941
_reflns_number_total             13345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034745ssi20030630_112819.cif
_cod_data_source_block           p96paps
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        11039(5)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4310402