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_4326210
_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            'C49 H55 Cu3 N38 O5.5 W2'
_chemical_formula_weight         1822.2
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_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     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             2011-01-10T12:56:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                70.8300(10)
_cell_angle_beta                 82.2460(10)
_cell_angle_gamma                82.4880(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8120(2)
_cell_length_b                   14.7920(3)
_cell_length_c                   21.6160(4)
_cell_measurement_reflns_used    13533
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3519.66(12)
_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 0.98
_diffrn_measured_fraction_theta_max 0.98
_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      0.0707569
_diffrn_orient_matrix_UB_12      0.034758
_diffrn_orient_matrix_UB_13      -0.0159626
_diffrn_orient_matrix_UB_21      0.02091
_diffrn_orient_matrix_UB_22      -0.0196361
_diffrn_orient_matrix_UB_23      0.0462002
_diffrn_orient_matrix_UB_31      0.0438056
_diffrn_orient_matrix_UB_32      -0.0597736
_diffrn_orient_matrix_UB_33      -0.0057385
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26592
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    4.22
_exptl_absorpt_correction_T_max  0.8494
_exptl_absorpt_correction_T_min  0.3198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_F_000             1787
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.831
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         15713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.073
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                11659
_reflns_number_total             15713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200689a_si_001_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        3519.66(11)
_cod_original_formula_sum        'C49 H55 Cu3 N38 O5.50 W2'
_cod_database_code               4326210