Tetra-Fe(iii) and deca-Mn(iii) metallacrowns built from bis-salicylhydrazide ligands: synthesis, structures and magnetic properties
Pan, Jia-li; Guo, Qian; Yang, Bing; Li, Yu-yi; Cao, Jin-ge; Meng, Xiang-gao; Xiao, Feng-ping; CrystEngComm 18 (2016) 6143–; doi:10.1039/C6CE01100D

data_7225820
_publ_section_title
;
 Tetra-Fe(iii) and deca-Mn(iii) metallacrowns built from
 bis-salicylhydrazide ligands: synthesis, structures and magnetic
 properties
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              6143
_journal_paper_doi               10.1039/C6CE01100D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C38 H32 Cl4 Fe4 N8 O16, 8(C3 H7 N O)'
_chemical_formula_sum            'C62 H88 Cl4 Fe4 N16 O24'
_chemical_formula_weight         1806.68
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-23 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.284(3)
_cell_length_b                   26.284(3)
_cell_length_c                   12.9228(15)
_cell_measurement_reflns_used    5316
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.45
_cell_measurement_theta_min      2.34
_cell_volume                     8927.7(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30373
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.844
_diffrn_reflns_theta_max         24.844
_diffrn_reflns_theta_min         1.549
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_correction_T_min  0.9216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, (Sheldrick,2008)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.087
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3857
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0607
_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^)+(0.1214P)^2^+30.6488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.2001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2880
_reflns_number_total             3857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01100d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7225820--7225823.cif.'
_cod_original_cell_volume        8928(2)
_cod_database_code               7225820
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              45557
_solvent_exptl_crystal_recrystallization_method 'DMF and Pyridine'