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_7043074
_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            'C152 H182 Cl4 F24 N22 Ni2 O44 Rh8 S8'
_chemical_formula_weight         4816.17
_chemical_name_common            4b
_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                90.1110(19)
_cell_angle_beta                 96.7631(18)
_cell_angle_gamma                93.5378(19)
_cell_formula_units_Z            1
_cell_length_a                   12.1474(5)
_cell_length_b                   18.7624(7)
_cell_length_c                   20.9552(8)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      66.74
_cell_measurement_theta_min      3.16
_cell_volume                     4733.5(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      170(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0814
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            74890
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        66.776
_diffrn_reflns_theta_max         66.776
_diffrn_reflns_theta_min         2.359
_exptl_absorpt_coefficient_mu    7.934
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       block
_exptl_crystal_F_000             2428
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvents (one dichloromethane, one methanol and one water 
 molecules) which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit them. 
;
_refine_diff_density_max         2.695
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         16356
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1212P)^2^+25.3938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11482
_reflns_number_total             16356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00836h2.cif
_cod_data_source_block           4b
_cod_database_code               7043074
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.300
_shelx_estimated_absorpt_t_max   0.382
_shelx_res_checksum              68428