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_7225823
_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         'C117 H106 Br10 Mn10 N26 O38'
_chemical_formula_sum            'C117 H106 Br10 Mn10 N26 O38'
_chemical_formula_weight         3832.77
_chemical_properties_physical    ', Air-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_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                113.598(6)
_cell_angle_beta                 91.571(7)
_cell_angle_gamma                95.727(6)
_cell_formula_units_Z            2
_cell_length_a                   20.239(9)
_cell_length_b                   21.285(9)
_cell_length_c                   26.335(11)
_cell_measurement_reflns_used    7588
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.11
_cell_measurement_theta_min      2.23
_cell_volume                     10316(8)
_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.1215
_diffrn_reflns_av_unetI/netI     0.1679
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16974
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        19.343
_diffrn_reflns_theta_max         19.343
_diffrn_reflns_theta_min         1.014
_exptl_absorpt_coefficient_mu    2.585
_exptl_absorpt_correction_T_max  0.7824
_exptl_absorpt_correction_T_min  0.6264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       needle
_exptl_crystal_F_000             3788
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_platon_squeeze_details
;
The total potential solvent accessible void volume is ca.  4300.7 Ang^3.
Electron Count per Cell is equal to 1884  which should be included 
in D(calc), F000 & Mol.Wght.

There are ca. twenty four DMF solvent molecules distributed to each 
coorination molecule according to the SQUEEZE/PLATON result.
;
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1654
_refine_ls_number_reflns         16974
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1638
_refine_ls_R_factor_gt           0.0989
_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^)+(0.1048P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2351
_refine_ls_wR_factor_ref         0.2597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8296
_reflns_number_total             16974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01100d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7225820--7225823.cif.'
_cod_database_code               7225823
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.926
_shelx_res_checksum              67592
_solvent_exptl_crystal_recrystallization_method 'DMF and Pyridine'