Self-assembled half-sandwich polyhedral cages via flexible Schiff-base ligands: an unusual macrocycle-to-cage conversion.
Liu, Jing-Jing; Lin, Yue-Jian; Li, Zhen-Hua; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13675–13679; doi:10.1039/c6dt02393b

data_7040040
_publ_section_title
;
 Self-assembled half-sandwich polyhedral cages via flexible Schiff-base
 ligands: an unusual macrocycle-to-cage conversion.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13675
_journal_page_last               13679
_journal_paper_doi               10.1039/c6dt02393b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C166 H228 Cl16 F24 N24 O43 Rh8 S8'
_chemical_formula_weight         5350.67
_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
_audit_update_record
;
2016-04-21 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.848(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9390(7)
_cell_length_b                   33.1198(13)
_cell_length_c                   36.5625(16)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.37
_cell_measurement_theta_min      2.94
_cell_volume                     21091.7(15)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.981
_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  0.0714
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            58929
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         2.489
_exptl_absorpt_coefficient_mu    8.387
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       block
_exptl_crystal_F_000             10848
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (half of a triflate anion, four 
 dichloromethane and one water molecules) which could not be 
 restrained properly. Therefore, SQUEEZE algorithm was used 
 to omit them. 
;
_refine_diff_density_max         3.563
_refine_diff_density_min         -2.298
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1245
_refine_ls_number_reflns         18856
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1590
_refine_ls_R_factor_gt           0.1470
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+2021.8409P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3532
_refine_ls_wR_factor_ref         0.3591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15604
_reflns_number_total             18856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02393b2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7040038--7040042.cif.'
_cod_database_code               7040040
_shelx_estimated_absorpt_t_min   0.134
_shelx_estimated_absorpt_t_max   0.285
_shelxl_version_number           2013-2
_shelx_res_checksum              48809