Self-assembly of tetranuclear {[Co(trien)]2[W(CN)8]2}2– or {[Co(tren)]2[W(CN)8]2}2– squares with alternating aliphatic tetramine Co(III) and octacyanotungstate(IV) corners
Kania, Rafał; Lewiński, Krzysztof; Sieklucka, Barbara; Dalton Transactions  (2003) 1033–1040; doi:10.1039/b210669h

data_7012400
_publ_section_title
;
 Self-assembly of tetranuclear {[Co(trien)]2[W(CN)8]2}2-- or
 {[Co(tren)]2[W(CN)8]2}2-- squares with alternating aliphatic tetramine
 Co(III) and octacyanotungstate(IV) corners
;
_journal_coden_ASTM              DTARAF
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              1033
_journal_page_last               1040
_journal_paper_doi               10.1039/b210669h
_journal_year                    2003
_chemical_formula_moiety
'(C6 H18 N4 Co 3+)2, (C8 N8 W 4+)2, (K 1+)2, (H2 O)9'
_chemical_formula_sum            'C28 H54 Co2 K2 N24 O9 W2'
_chemical_formula_weight         1434.72
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.7700(8)
_cell_angle_beta                 83.4290(7)
_cell_angle_gamma                88.5950(6)
_cell_formula_units_Z            2
_cell_length_a                   11.7830(2)
_cell_length_b                   13.0640(2)
_cell_length_c                   16.4650(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2507.12(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans with the \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21401
_diffrn_reflns_theta_full        29.66
_diffrn_reflns_theta_max         29.66
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    5.460
_exptl_absorpt_correction_T_max  0.6113
_exptl_absorpt_correction_T_min  0.4081
_exptl_absorpt_correction_type
'multi-scan (DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         8.082
_refine_diff_density_min         -3.497
_refine_diff_density_rms         0.430
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         14037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0978
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+50.6314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2612
_refine_ls_wR_factor_ref         0.2745
_reflns_number_gt                11087
_reflns_number_total             14037
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210669h.txt
_cod_data_source_block           kco
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+50.6314P] 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^)+(0.1312P)^2^+50.6314P] 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        2507.12(6)
_cod_original_formula_sum        'C28 H54 N24 O9 Co2 K2 W2'
_cod_database_code               7012400