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_7040039
_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            'C124 H138 F24 N20 O28 Rh6 S8'
_chemical_formula_weight         3686.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-07 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.740(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.658(17)
_cell_length_b                   25.83(2)
_cell_length_c                   34.51(3)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.912
_cell_measurement_theta_min      2.378
_cell_volume                     17363(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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            121608
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         0.988
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             7440
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvent (four triflate anions and one 
 acetonitrile molecule) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         2.794
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1799
_refine_ls_number_reflns         37739
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0839
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1622P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2370
_refine_ls_wR_factor_ref         0.2634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20867
_reflns_number_total             37739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02393b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7040038--7040042.cif.'
_cod_original_cell_volume        17365(27)
_cod_database_code               7040039
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.808
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              61662