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_7043077
_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            'C154 H180 F24 N24 O42 Pd2 Rh8 S8'
_chemical_formula_weight         4787.77
_chemical_name_common            5b
_chemical_name_systematic
; 
 ? 
;
_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-2013
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2017-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                89.3467(16)
_cell_angle_beta                 83.4094(17)
_cell_angle_gamma                86.6129(16)
_cell_formula_units_Z            1
_cell_length_a                   12.0423(5)
_cell_length_b                   18.7950(7)
_cell_length_c                   21.1589(8)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.46
_cell_measurement_theta_min      2.35
_cell_volume                     4749.0(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.975
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60888
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.497
_diffrn_reflns_theta_min         3.150
_exptl_absorpt_coefficient_mu    8.663
_exptl_absorpt_correction_T_max  0.226
_exptl_absorpt_correction_T_min  0.067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       prism
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (one triflate anion, one methanol and 
 one acetonitrile molecules) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         2.128
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         17397
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0832
_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^)+(0.0831P)^2^+52.9564P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14388
_reflns_number_total             17397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00836h2.cif
_cod_data_source_block           5b
_cod_database_code               7043077
_shelx_estimated_absorpt_t_min   0.221
_shelx_estimated_absorpt_t_max   0.305
_shelxl_version_number           2013-2
_shelx_res_checksum              59389