Radical-Copper Wheels: Structure and Magnetism of Hexanuclear Hybrid Arrays
Junichi Omata; Takayuki Ishida; Daisuke Hashizume; Fujiko Iwasaki; Takashi Nogami; Inorganic Chemistry 40 (2001) 3954–3958; doi:10.1021/ic001462g

data_4320017
_publ_contact_author
;
    Takayuki ISHIDA
    Department of Applied Physics and Chemistry, The University of 
    Electro-Communications, Chofu, Tokyo 182-8585, Japan
;
_publ_contact_author_email       'ishi@pc.uec.ac.jp '
_publ_contact_author_fax         ' +81 424 43 5501 '
_publ_contact_author_phone       ' +81 424 43 5490 '
_publ_section_title
;
 Radical-Copper Wheels: Structure and Magnetism of Hexanuclear Hybrid
 Arrays
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3954
_journal_page_last               3958
_journal_paper_doi               10.1021/ic001462g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C11 H15 Br2 Cu N4 O2, 0.3(H2 O)'
_chemical_formula_sum            'C11 H15.6 Br2 Cu N4 O2.3'
_chemical_formula_weight         464.02
_chemical_name_systematic
; 
 Dibromo(4-pyrimidinylnitronylnitroxide)copper(II)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   28.172(2)
_cell_length_b                   28.172(2)
_cell_length_c                   12.590(2)
_cell_measurement_reflns_used    18092
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     8653.5(16)
_computing_cell_refinement       'Rapid Auto (Higashi, 1998)'
_computing_data_collection       'Rapid Auto (Higashi, 1998)'
_computing_data_reduction        'Rapid Auto (Higashi, 1998)'
_computing_molecular_graphics    'SV (Nemoto & Ohashi, 1993)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI 91 (Hai-Fu, 1991)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.154
_diffrn_reflns_av_sigmaI/netI    0.3624
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25081
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    5.298
_exptl_absorpt_correction_T_max  0.8423
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numabs - Numerical absorption correction based on 
 crystal shape (Higashi, T, 1999).
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4092
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.716
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4407
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.715
_refine_ls_R_factor_all          0.2323
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1319
_reflns_number_gt                1230
_reflns_number_total             4407
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic001462g.cif
_cod_data_source_block           '[Cu(4-PMNN)Br_2]'
_cod_original_cell_volume        8653(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4320017