Nano-sized heterometallic macrocycles based on 4-pyridinylboron-capped iron(II) clathrochelates: syntheses, structures and properties
Ying-Ying Zhang; Yue-Jian Lin; Guo-Xin Jin; Chem.Commun. 50 (2014) 2327–; doi:10.1039/c3cc49038f

data_7112007
_publ_section_title
;
 Nano-sized heterometallic macrocycles based on 4-pyridinylboron-capped
 iron(II) clathrochelates: syntheses, structures and properties
;
_journal_name_full               Chem.Commun.
_journal_page_first              2327
_journal_paper_doi               10.1039/c3cc49038f
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C52 H70 B2 Cl12 Fe Ir2 N8 O6'
_chemical_formula_weight         1790.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                106.900(3)
_cell_angle_beta                 90.895(4)
_cell_angle_gamma                93.715(4)
_cell_formula_units_Z            2
_cell_length_a                   10.557(2)
_cell_length_b                   16.941(4)
_cell_length_c                   20.082(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3427.0(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0950
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20021
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    4.601
_exptl_absorpt_correction_T_max  0.7389
_exptl_absorpt_correction_T_min  0.4597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.097
_refine_diff_density_min         -2.496
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         11925
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.2108
_reflns_number_gt                8233
_reflns_number_total             11925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc49038f.txt
_cod_data_source_block           mo30321a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7112007