Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged CuIILnIII and NiII(Low-Spin)LnIII Compounds Derived from a Compartmental Ligand (Ln = Ce-Yb)
Arpita Jana; Samit Majumder; Luca Carrella; Malabika Nayak; Thomas Weyhermueller; Supriya Dutta; Dieter Schollmeyer; Eva Rentschler; Rajesh Koner; Sasankasekhar Mohanta; Inorganic Chemistry 49 (2010) 9012–9025; doi:10.1021/ic101445n

data_4316668
_publ_section_title
;
 Syntheses, Structures, and Magnetic Properties of Diphenoxo-Bridged
 CuIILnIII and NiII(Low-Spin)LnIII Compounds Derived from a Compartmental
 Ligand (Ln = Ce-Yb)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9012
_journal_page_last               9025
_journal_paper_doi               10.1021/ic101445n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C24 H28 Cu N5 O13 Yb'
_chemical_formula_weight         831.1
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.290(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5876(3)
_cell_length_b                   25.2526(9)
_cell_length_c                   13.2704(5)
_cell_measurement_reflns_used    5218
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.2
_cell_volume                     2831.52(18)
_computing_cell_refinement       'Enraf Nonius Software V5'
_computing_data_collection       'Enraf Nonius Software V5'
_computing_data_reduction        'Corinc (Dr\"ager, 1971)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Smart CCD'
_diffrn_measurement_method       'CCD scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_sigmaI/netI    0.0928
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28494
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.54
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.110
_exptl_absorpt_correction_T_max  0.525
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Mulabs (Blessing)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.269
_refine_diff_density_min         -1.066
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0800
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                4351
_reflns_number_total             7009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101445n_si_001_08.cif
_cod_data_source_block           12
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C24 H28 Cu1 N5 O13 Yb1'
_cod_database_code               4316668