Family of Mixed 3d-4f Dimeric 14-Metallacrown-5 Compounds: Syntheses, Structures, and Magnetic Properties
Fan Cao; Suna Wang; Dacheng Li; Suyuan Zeng; Meiju Niu; You Song; Jianmin Dou; Inorganic Chemistry 52 (2013) 10747–10755; doi:10.1021/ic3025952

data_4336118
_publ_section_title
;
 Family of Mixed 3d-4f Dimeric 14-Metallacrown-5 Compounds: Syntheses,
 Structures, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10747
_journal_page_last               10755
_journal_paper_doi               10.1021/ic3025952
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C86 H128 Cl8 Gd4 Mn8 N8 O64'
_chemical_formula_weight         3650.08
_chemical_name_systematic
; 
 ? 
;
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_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                80.8060(10)
_cell_angle_beta                 79.8670(10)
_cell_angle_gamma                83.792(2)
_cell_formula_units_Z            1
_cell_length_a                   12.9985(11)
_cell_length_b                   13.0134(12)
_cell_length_c                   20.455(2)
_cell_measurement_reflns_used    5079
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.088
_cell_measurement_theta_min      2.345
_cell_volume                     3350.9(5)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16867
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    2.927
_exptl_absorpt_correction_T_max  0.6208
_exptl_absorpt_correction_T_min  0.4543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_description       block
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.805
_refine_diff_density_min         -2.521
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         11638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0617P)^2^+11.4029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                7308
_reflns_number_total             11638
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3025952_si_003.cif
_cod_data_source_block           120808c
_cod_original_cell_volume        3350.8(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4336118