Bimetallic M(V)(2)Cu(II)(3) (M = Mo, W) coordination complexes based on octacyanometalates: structures and magnetic variations tuned by chelated tetradentate macrocyclic ligands.
Lim, Jeong Hak; You, Young Sin; Yoo, Houng Sik; Yoon, Jung Hee; Kim, Jae Il; Koh, Eui Kwan; Hong, Chang Seop; Inorganic chemistry 46 (2007) 10578–10586; doi:10.1021/ic701243w

data_4339303
_publ_section_title
;
 Bimetallic M(V)(2)Cu(II)(3) (M = Mo, W) coordination complexes based on
 octacyanometalates: structures and magnetic variations tuned by chelated
 tetradentate macrocyclic ligands.
;
_journal_issue                   25
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10578
_journal_page_last               10586
_journal_paper_doi               10.1021/ic701243w
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C46 H82 Cu3 N28 O5 W2'
_chemical_formula_weight         1665.72
_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_creation_method           SHELXL-97
_cell_angle_alpha                78.342(5)
_cell_angle_beta                 83.074(5)
_cell_angle_gamma                69.472(5)
_cell_formula_units_Z            1
_cell_length_a                   8.9255(11)
_cell_length_b                   10.0938(13)
_cell_length_c                   19.549(3)
_cell_measurement_reflns_used    5342
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.903
_cell_measurement_theta_min      2.287
_cell_volume                     1613.0(4)
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_collection       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21064
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    4.590
_exptl_absorpt_correction_T_max  0.8746
_exptl_absorpt_correction_T_min  0.6568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             829
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.657
_refine_diff_density_min         -2.323
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0693
_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^)+(0.1037P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1779
_reflns_number_gt                5870
_reflns_number_total             7570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701243w-file001.cif
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4339303