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_7043076
_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            'C148 H178 Cl8 F24 N26 Ni2 O24 Rh8 S8'
_chemical_formula_weight         4641.93
_chemical_name_common            4a
_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                89.438(3)
_cell_angle_beta                 83.265(3)
_cell_angle_gamma                83.267(3)
_cell_formula_units_Z            1
_cell_length_a                   11.9791(7)
_cell_length_b                   19.0988(10)
_cell_length_c                   21.5260(11)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.69
_cell_measurement_theta_min      3.12
_cell_volume                     4857.1(5)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.915
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       14
_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            40973
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        66.869
_diffrn_reflns_theta_max         66.869
_diffrn_reflns_theta_min         2.329
_exptl_absorpt_coefficient_mu    8.128
_exptl_absorpt_correction_T_max  0.219
_exptl_absorpt_correction_T_min  0.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       rod
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvent (one triflate anion and one acetonitrile 
 molecule) which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit them. 
;
_refine_diff_density_max         1.991
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         15800
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1278
_refine_ls_R_factor_gt           0.1035
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1365P)^2^+56.3296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2789
_refine_ls_wR_factor_ref         0.2944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10998
_reflns_number_total             15800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00836h2.cif
_cod_data_source_block           4a
_cod_database_code               7043076
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.181
_shelx_estimated_absorpt_t_max   0.641
_shelx_res_checksum              90988