The Encapsulation of Ferrocyanide by Copper(II) Complexes of Tripodal Tetradentate Ligands. Novel H-Bonding Networks Incorporating Heptanuclear and Pentanuclear Heterometallic Assemblies
Richard J. Parker; Leone Spiccia; Stuart R. Batten; John D. Cashion; Gary D. Fallon; Inorganic Chemistry 40 (2001) 4696–4704; doi:10.1021/ic001452f

data_4320162
_publ_contact_author
;
    Dr. Leone Spiccia
    School of Chemistry
    PO Box 23
    Monash University 3800
    AUSTRALIA
;
_publ_contact_author_email       'leone.spiccia@sci.monash.edu.au '
_publ_contact_author_fax         ' +61 3 9905 4597 '
_publ_contact_author_phone       ' +61 3 9905 4526 '
_publ_section_title
;
 The Encapsulation of Ferrocyanide by Copper(II) Complexes of Tripodal
 Tetradentate Ligands. Novel H-Bonding Networks Incorporating Heptanuclear
 and Pentanuclear Heterometallic Assemblies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4696
_journal_page_last               4704
_journal_paper_doi               10.1021/ic001452f
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C108 H258 Cu10 Fe6 N76 O27 S6'
_chemical_formula_weight         4216.76
_chemical_name_common
'[{Cu(tren)CN}6Fe][{Cu(tren)CN}4Fe(CN)2][Fe(CN)6]4.6DMSO.21H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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
_cell_angle_alpha                110.750(3)
_cell_angle_beta                 90.206(2)
_cell_angle_gamma                112.754(3)
_cell_formula_units_Z            1
_cell_length_a                   14.8094(8)
_cell_length_b                   17.3901(7)
_cell_length_c                   21.1565(11)
_cell_measurement_reflns_used    40966
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      1.04
_cell_volume                     4635.7(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       phi-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  0.085
_diffrn_reflns_av_sigmaI/netI    0.1941
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40966
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    1.719
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.799
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         33143
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1975
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.633
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+6.0864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2512
_reflns_number_gt                16884
_reflns_number_total             33143
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001452f_2.cif
_cod_data_source_block           rp1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+6.0864P] 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^)+(0.1154P)^2^+6.0864P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320162