Design and self-assembly of variform organometallic macrocycle with terminal imidazole-based bridging ligands utilizing joints twist and rotation.
Wu, Tong; Lin, Yue-Jian; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2356–2360; doi:10.1039/c3dt52724g

data_7028794
_publ_section_title
;
 Design and self-assembly of variform organometallic macrocycle with
 terminal imidazole-based bridging ligands utilizing joints twist and
 rotation.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2356
_journal_page_last               2360
_journal_paper_doi               10.1039/c3dt52724g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C84 H116 F6 Ir2 N8 O14 S2'
_chemical_formula_weight         2024.36
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 123.0740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.2926(8)
_cell_length_b                   16.2805(4)
_cell_length_c                   28.4835(6)
_cell_measurement_reflns_used    4418
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      58.31
_cell_measurement_theta_min      2.91
_cell_volume                     14102.8(6)
_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 0.950
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35496
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.997
_diffrn_reflns_theta_min         2.906
_exptl_absorpt_coefficient_mu    8.565
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       block
_exptl_crystal_F_000             8224
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
; 
 In asymmetric unit of 3a, there were disordered solvents 
 (three diethyl ether and four methanol molecules) which 
 could not be restrained properly. Therefore, SQUEEZE 
 algorithm was used to omit them. 
;
_refine_diff_density_max         4.182
_refine_diff_density_min         -3.328
_refine_diff_density_rms         0.389
_refine_ls_extinction_coef       0.000104(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         12189
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1715P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9859
_reflns_number_total             12189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt52724g.txt
_cod_data_source_block           3a
_cod_database_code               7028794
_shelx_estimated_absorpt_t_min   0.627
_shelx_estimated_absorpt_t_max   0.783
_shelxl_version_number           2013-2
_shelx_res_checksum              87112
_shelx_hkl_checksum              54633