Supramolecular metallomacrocycles based on trans-dicyanoferrite(III) building blocks: synthesis, crystal structure and magnetic properties
Ni, Zhong-Hai; Tao, Jun; Wernsdorfer, Wolfgang; Cui, Ai-Li; Kou, Hui-Zhong; Dalton Transactions  (2009) 2788–2794; doi:10.1039/b814860k

data_7030533
_publ_section_title
;
 Supramolecular metallomacrocycles based on trans-dicyanoferrite(III)
 building blocks: synthesis, crystal structure and magnetic properties
;
_journal_coden_ASTM              DTARAF
_journal_issue                   15
_journal_name_full               'Dalton Transactions'
_journal_page_first              2788
_journal_page_last               2794
_journal_paper_doi               10.1039/b814860k
_journal_year                    2009
_chemical_formula_sum            'C38 H33 Cl Fe Mn N8 O6'
_chemical_formula_weight         843.96
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.16150(10)
_cell_length_b                   23.16150(10)
_cell_length_c                   15.18050(10)
_cell_measurement_reflns_used    4780
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      3.09
_cell_volume                     8143.66(7)
_computing_cell_refinement       'crystalstructure 3.6.0 (Rigaku/MSC, 2004)'
_computing_data_collection       'crystalstructure 3.6.0 (Rigaku/MSC, 2004)'
_computing_data_reduction        'Crystalstructure 2004'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XP (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.77
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Rigaku IP'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7548
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR; Higashi, 1995'
_exptl_crystal_colour            'red brown'
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         7548
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+2.0016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1777
_reflns_number_gt                4780
_reflns_number_total             7548
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7000977
_cod_data_source_file            b814860k.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-42(1)c
_cod_database_code               7030533