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_7112006
_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            'C194 H270 B4 Cl12 F12 Fe2 Ir4 N24 O27 S4'
_chemical_formula_weight         5075.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 94.1160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   58.688(4)
_cell_length_b                   21.7043(16)
_cell_length_c                   17.5541(13)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.23
_cell_volume                     22302(3)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            67613
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         0.70
_diffrn_standards_decay_%        5.35
_exptl_absorpt_coefficient_mu    2.763
_exptl_absorpt_correction_T_max  0.8742
_exptl_absorpt_correction_T_min  0.7328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sheet
_exptl_crystal_F_000             10296
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_platon_squeeze_details          ' '
_refine_diff_density_max         4.609
_refine_diff_density_min         -2.256
_refine_diff_density_rms         0.272
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.499(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2298
_refine_ls_number_reflns         36117
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2010
_refine_ls_wR_factor_ref         0.2198
_reflns_number_gt                27002
_reflns_number_total             36117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc49038f.txt
_cod_data_source_block           mo_30318a
_cod_original_cell_volume        22303(3)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7112006