Microwave-Assisted Construction of Ferromagnetic Coordination Polymers of [WV(CN)8]3- with CuII-pyrazole Synthons
Olaf Stefanczyk; Tomasz Korzeniak; Wojciech Nitek; Michał Rams; Barbara Sieklucka; Inorganic Chemistry 50 (2011) 8808–8816; doi:10.1021/ic200689a

data_4326209
_publ_section_title
;
 Microwave-Assisted Construction of Ferromagnetic Coordination Polymers of
 [WV(CN)8]3- with CuII-pyrazole Synthons
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8808
_journal_page_last               8816
_journal_paper_doi               10.1021/ic200689a
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C56 H46 Cu4 N28 O11 W2'
_chemical_formula_sum            'C96 H106 Cu8 N72 O19 W4'
_chemical_formula_weight         3815.44
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_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             2011-02-15T10:22:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                61.9300(10)
_cell_angle_beta                 87.2970(10)
_cell_angle_gamma                87.6650(10)
_cell_formula_units_Z            1
_cell_length_a                   14.7530(2)
_cell_length_b                   16.5290(2)
_cell_length_c                   16.6930(3)
_cell_measurement_reflns_used    14796
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     3587.02(10)
_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-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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      -0.159103E-1
_diffrn_orient_matrix_UB_12      0.292003E-1
_diffrn_orient_matrix_UB_13      -0.654354E-1
_diffrn_orient_matrix_UB_21      -0.648362E-1
_diffrn_orient_matrix_UB_22      -0.169245E-1
_diffrn_orient_matrix_UB_23      0.182144E-1
_diffrn_orient_matrix_UB_31      -0.122391E-1
_diffrn_orient_matrix_UB_32      0.596985E-1
_diffrn_orient_matrix_UB_33      0.5328E-3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28457
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.38
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.434
_exptl_absorpt_correction_T_max  0.4036
_exptl_absorpt_correction_T_min  0.3497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       prism
_exptl_crystal_F_000             1865
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.245
_refine_diff_density_min         -1.635
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         16288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+9.7367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                13112
_reflns_number_total             16288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200689a_si_001_2.cif
_cod_data_source_block           3
_cod_original_cell_volume        3587.02(9)
_cod_database_code               4326209