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_4320161
_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            'C54 H139.6 Cl2 Cu6 Fe3 N42 O23.8'
_chemical_formula_weight         2378.17
_chemical_name_common            '[{Cu(tren)CN}6Fe}{Fe(CN)6]2[ClO4]2.16H20'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.8300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8674(10)
_cell_length_b                   25.9587(10)
_cell_length_c                   27.5617(10)
_cell_measurement_reflns_used    120529
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      1.09
_cell_volume                     10447.7(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.102
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            120529
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    1.73
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             4936
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.904
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         19085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1722
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          1.881
_refine_ls_shift/su_mean         0.177
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1873P)^2^+66.0991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2694
_refine_ls_wR_factor_ref         0.3297
_reflns_number_gt                11181
_reflns_number_total             19085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001452f_1.cif
_cod_data_source_block           k077a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1873P)^2^+66.0991P] 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^)+(0.1873P)^2^+66.0991P] 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               4320161