Eicosanuclear Cluster [Cu13W7] of Copper-Octacyanotungstate Bimetallic Assembly: Synthesis, Structure, and Magnetic Properties
Jun Wang; Zai-Chao Zhang; Hui-Sheng Wang; Ling-Chen Kang; Hong-Bo Zhou; You Song; Xiao-Zeng You; Inorganic Chemistry 49 (2010) 3101–3103; doi:10.1021/ic100282w

data_4315267
_publ_section_title
;
 Eicosanuclear Cluster [Cu13W7] of Copper-Octacyanotungstate Bimetallic
 Assembly: Synthesis, Structure, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3101
_journal_page_last               3103
_journal_paper_doi               10.1021/ic100282w
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
;
C164 H254 Cu13 N92 O W7, 3.2(H4 O2), 8(H1.20 O0.60),
 16(H0.80 O0.40), 16(H0.80 O0.40) 
;
_chemical_formula_sum            'C164 H302 Cu13 N92 O25 W7'
_chemical_formula_weight         6076.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           107
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4 -2'
_symmetry_space_group_name_H-M   'I 4 m m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   31.2762(12)
_cell_length_b                   31.2762(12)
_cell_length_c                   16.1133(18)
_cell_measurement_reflns_used    5678
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      23.02
_cell_measurement_theta_min      2.35
_cell_volume                     15762(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega 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  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43299
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    3.454
_exptl_absorpt_correction_T_max  0.501
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6050
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.727
_refine_diff_density_min         -1.894
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         8220
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.06P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                6642
_reflns_number_total             8220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100282w_si_002.cif
_cod_data_source_block           Cu13W7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 
;
_cod_original_sg_symbol_Hall     'I 4 -2 '
_cod_original_sg_symbol_H-M      'I 4 m m '
_cod_database_code               4315267