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_4326208
_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_formula_sum            'C23 H24 Cu2 N19 O5 W'
_chemical_formula_weight         957.54
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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             2010-10-21T23:49:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.5050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.0150(6)
_cell_length_b                   14.6360(3)
_cell_length_c                   15.4030(3)
_cell_measurement_reflns_used    15559
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6991.7(2)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_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
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0125817
_diffrn_orient_matrix_UB_12      0.0292168
_diffrn_orient_matrix_UB_13      -0.0527142
_diffrn_orient_matrix_UB_21      0.0230763
_diffrn_orient_matrix_UB_22      0.0284433
_diffrn_orient_matrix_UB_23      0.036818
_diffrn_orient_matrix_UB_31      0.018678
_diffrn_orient_matrix_UB_32      -0.0548218
_diffrn_orient_matrix_UB_33      -0.0089913
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28629
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    4.551
_exptl_absorpt_correction_T_max  0.5485
_exptl_absorpt_correction_T_min  0.2633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.724
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.00021(2)
_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   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0420P)^2^+4.0220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.071
_refine_ls_wR_factor_ref         0.0755
_reflns_number_gt                6544
_reflns_number_total             7991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200689a_si_001_1.cif
_cod_data_source_block           1
_cod_database_code               4326208