Box-like Heterometallic Macrocycles Derived from Bis-Terpyridine Metalloligands
Liu, Jing-Jing; Lin, Yue-Jian; Jin, Guo-Xin; Organometallics 33 (2014) 1283–; doi:10.1021/om500093p

data_4082781
_publ_section_title
;
 Box-like Heterometallic Macrocycles Derived from Bis-Terpyridine
 Metalloligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1283
_journal_paper_doi               10.1021/om500093p
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C200 H238 F48 Ir4 N26 O22 Sb8 Zn2'
_chemical_formula_weight         6143.69
_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                 108.671(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.5442(18)
_cell_length_b                   26.968(3)
_cell_length_c                   25.609(3)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      2.27
_cell_volume                     11479(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0880
_diffrn_reflns_av_unetI/netI     0.1206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            83628
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         1.129
_exptl_absorpt_coefficient_mu    3.541
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       block
_exptl_crystal_F_000             6008
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvent molecules (two diethyl ether, three acetonitrile 
 and four water molecules) which could not restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         9.267
_refine_diff_density_min         -2.857
_refine_diff_density_rms         0.351
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1173
_refine_ls_number_reflns         26423
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1715
_refine_ls_R_factor_gt           0.1152
_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^)+(0.2000P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3143
_refine_ls_wR_factor_ref         0.3425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13575
_reflns_number_total             26423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500093p_si_002.cif
_cod_data_source_block           1a'
_cod_database_code               4082781
_shelx_estimated_absorpt_t_min   0.790
_shelx_estimated_absorpt_t_max   0.901
_shelxl_version_number           2013-2
_shelx_res_checksum              56812
_shelx_hkl_checksum              17538