Syntheses, Structures and Magnetic Properties of Lanthanide Complexes of the Pyrimidyl-Substituted Nitronyl Nitroxide Radical
Wang, Jian; Miao, Hao; Xiao, Zhao-Xin; Zhou, Yan; Deng, Lin-Dan; Zhang, Yiquan; Wang, Xin-Yi; Dalton Trans.  (2017) –; doi:10.1039/C7DT01037K

data_7043625
_publ_section_title
;
 Syntheses, Structures and Magnetic Properties of Lanthanide Complexes of
 the Pyrimidyl-Substituted Nitronyl Nitroxide Radical
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01037K
_journal_year                    2017
_chemical_formula_sum            'C44.5 H33 F36 N4 O16 Tb2'
_chemical_formula_weight         1881.59
_chemical_name_common            '[(NIT-2-Pm)(Tb)2(hfac)6(H2O)2]0.5(C7H16)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-28 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.3960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.622(3)
_cell_length_b                   24.365(3)
_cell_length_c                   23.015(4)
_cell_measurement_reflns_used    5516
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.79
_cell_measurement_theta_min      2.23
_cell_volume                     13079(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1356
_diffrn_reflns_av_unetI/netI     0.1421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57842
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         1.209
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            PURPLE
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             7280
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_refine_diff_density_max         2.061
_refine_diff_density_min         -1.677
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     950
_refine_ls_number_reflns         15039
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9263
_reflns_number_total             15039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01037k4.cif
_cod_data_source_block           1538979
_cod_original_formula_sum        'C44.50 H33 F36 N4 O16 Tb2'
_cod_database_code               7043625
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.630
_shelx_estimated_absorpt_t_max   0.753
_shelx_res_checksum              58277
_shelx_fab_checksum              17515