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_7112008
_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            'C46 H64 B2 Cl12 Fe Ir2 N8 O6'
_chemical_formula_weight         1712.32
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.4350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9176(11)
_cell_length_b                   19.1802(14)
_cell_length_c                   23.1519(17)
_cell_measurement_reflns_used    9382
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.27
_cell_volume                     6415.2(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            42071
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.249
_diffrn_reflns_theta_min         1.410
_exptl_absorpt_coefficient_mu    4.911
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       block
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.028
_refine_diff_density_min         -1.983
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         12888
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+20.8266P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11158
_reflns_number_total             12888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc49038f.txt
_cod_data_source_block           mo_30916c
_cod_database_code               7112008
_shelx_estimated_absorpt_t_min   0.507
_shelx_estimated_absorpt_t_max   0.828
_shelxl_version_number           2013-2
_shelx_res_checksum              92589
_shelx_hkl_checksum              37188