W-Knotted Chain {[CuII(dien)]4[WV(CN)8]}5+\ιnfty: Synthesis, Crystal Structure, Magnetism, and Theory
Robert Podgajny; Robert Pełka; Cédric Desplanches; Laurent Ducasse; Wojciech Nitek; Tomasz Korzeniak; Olaf Stefanczyk; Michał Rams; Barbara Sieklucka; Michel Verdaguer; Inorganic Chemistry 50 (2011) 3213–3222; doi:10.1021/ic101335a

data_4324826
_publ_section_title
;
 W-Knotted Chain {[CuII(dien)]4[WV(CN)8]}5+\\infty: Synthesis, Crystal
 Structure, Magnetism, and Theory
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3213
_journal_page_last               3222
_journal_paper_doi               10.1021/ic101335a
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H70 Cu3 N34 W2'
_chemical_formula_sum            'C40 H32 Cu4 N36 O10.5 W3'
_chemical_formula_weight         1990.73
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      85
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2011-01-24T13:37:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2059(3)
_cell_length_b                   24.2059(3)
_cell_length_c                   13.3200(2)
_cell_measurement_reflns_used    17891
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     7804.53(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.393547E-1
_diffrn_orient_matrix_UB_12      -0.8513E-2
_diffrn_orient_matrix_UB_13      0.168585E-1
_diffrn_orient_matrix_UB_21      0.8471E-2
_diffrn_orient_matrix_UB_22      -0.46273E-2
_diffrn_orient_matrix_UB_23      -0.729976E-1
_diffrn_orient_matrix_UB_31      0.93204E-2
_diffrn_orient_matrix_UB_32      0.401511E-1
_diffrn_orient_matrix_UB_33      -0.48384E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.06
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            43461
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.538
_exptl_absorpt_correction_T_max  0.6074
_exptl_absorpt_correction_T_min  0.2154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       prism
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         7.539
_refine_diff_density_min         -3.548
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    71.283
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         8294
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+128.0444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2152
_reflns_number_gt                6151
_reflns_number_total             8294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101335a_si_002.cif
_cod_data_source_block           os81
_cod_original_cell_volume        7804.50(18)
_cod_original_sg_symbol_Hall     P4ab-1ab
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_original_formula_sum        'C40 H32 Cu4 N36 O10.50 W3'
_cod_database_code               4324826