Synthesis, Crystal Structures, and Magnetic Properties of Cyano-Bridged Honeycomblike Layers MV−CuII(M = Mo, W) Chelated by a Macrocyclic Ligand
Lim, Jeong Hak; Kang, Jun Sung; Kim, Hyoung Chan; Koh, Eui Kwan; Hong, Chang Seop; Inorganic Chemistry 45 (2006) 7821–7827; doi:10.1021/ic060868b

data_4332813
_publ_section_title
;
 Synthesis, Crystal Structures, and Magnetic Properties of Cyano-Bridged
 Honeycomblike Layers MV&#x2212;CuII(M = Mo, W) Chelated by a Macrocyclic
 Ligand
;
_journal_issue                   19
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7821
_journal_page_last               7827
_journal_paper_doi               10.1021/ic060868b
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C42 H76 Cu1.5 Mo N14 O4'
_chemical_formula_weight         1032.42
_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                74.3290(10)
_cell_angle_beta                 86.3890(10)
_cell_angle_gamma                78.1000(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3001(2)
_cell_length_b                   16.3346(4)
_cell_length_c                   16.4319(4)
_cell_measurement_temperature    130
_cell_volume                     2604.59(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41992
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.899
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1087
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.652
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         12715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+5.0758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                10534
_reflns_number_total             12715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060868bsup2.cif
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      p-1
_cod_original_formula_sum        'C42 H76 Cu1.50 Mo N14 O4'
_cod_database_code               4332813