Controllable Construction of Half-sandwich Octanuclear Cages Based on Pyridyl-substituted Ligands with Conjugated Centers
Jin, Guo-Xin; Guo, Bei-Bei; Lin, Yue-Jian; Dalton Trans.  (2017) –; doi:10.1039/C7DT00836H

data_7043075
_publ_section_title
;
 Controllable Construction of Half-sandwich Octanuclear Cages Based on
 Pyridyl-substituted Ligands with Conjugated Centers
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00836H
_journal_year                    2017
_chemical_formula_sum            'C164 H184 Cl8 F24 N8 O30 Rh8 S8'
_chemical_formula_weight         4566.54
_chemical_name_common            6
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                104.18(2)
_cell_angle_beta                 94.641(13)
_cell_angle_gamma                100.406(14)
_cell_formula_units_Z            1
_cell_length_a                   12.4501(15)
_cell_length_b                   19.268(5)
_cell_length_c                   21.042(3)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.02
_cell_measurement_theta_min      2.79
_cell_volume                     4771.8(16)
_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 0.906
_diffrn_measured_fraction_theta_max 0.906
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.906
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49252
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        67.493
_diffrn_reflns_theta_max         67.493
_diffrn_reflns_theta_min         2.184
_exptl_absorpt_coefficient_mu    8.076
_exptl_absorpt_correction_T_max  0.322
_exptl_absorpt_correction_T_min  0.149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       rod
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (two and a half triflate anions, two 
 methanol and one water molecules) which could not be 
 restrained properly. Therefore, SQUEEZE algorithm was used 
 to omit them. 
;
_refine_diff_density_max         3.912
_refine_diff_density_min         -2.927
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         15567
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.1126
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+120.3857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2970
_refine_ls_wR_factor_ref         0.3021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12492
_reflns_number_total             15567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00836h2.cif
_cod_data_source_block           6
_cod_original_cell_volume        4771.9(15)
_cod_database_code               7043075
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.159
_shelx_estimated_absorpt_t_max   0.738
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              4702