Synthesis, Structures and Magnetic Properties of Chiral 3d-3d'-4f Heterotrimetallic Complexes Based on [(Tp*)Fe(CN)3]-
Deng, Xiao-Wei; Cai, Li-Zheng; Zhu, Zhao-Xia; Gao, Feng; Zhou, Yanling; Yao, Min-Xia; New J. Chem. 41 (2017) 5988–5994; doi:10.1039/C7NJ01413A

data_7056244
_publ_section_title
;
 Synthesis, Structures and Magnetic Properties of Chiral 3d-3d'-4f
 Heterotrimetallic Complexes Based on [(Tp*)Fe(CN)3]-&#xF02D;
;
_journal_issue                   13
_journal_name_full               'New J. Chem.'
_journal_page_first              5988
_journal_page_last               5994
_journal_paper_doi               10.1039/C7NJ01413A
_journal_volume                  41
_journal_year                    2017
_chemical_absolute_configuration S
_chemical_formula_sum            'C58 H74 B2 Cu Fe2 N21 O10 Tb'
_chemical_formula_weight         1581.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-27 deposited with the CCDC.
2017-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.2710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5669(13)
_cell_length_b                   16.1004(16)
_cell_length_c                   17.8246(18)
_cell_measurement_reflns_used    4884
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.82
_cell_measurement_theta_min      2.49
_cell_volume                     3789.5(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0976
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20208
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.726
_exptl_absorpt_coefficient_mu    1.637
_exptl_crystal_colour            'BLACK RED'
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1610
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.013(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         12803
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.929
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9657
_reflns_number_total             12803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01413a2.cif
_cod_data_source_block           2-SS
_cod_database_code               7056244
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.757
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              26314