Rational Design of Polynuclear Organometallic Assemblies from a Simple Heteromultifunctional Ligand.
Zhang, Long; Lin, Yue-Jian; Li, Zhen-Hua; Jin, Guo-Xin; Journal of the American Chemical Society 137 (2015) 13670–13678; doi:10.1021/jacs.5b08826

data_4129615
_publ_section_title
;
 Rational Design of Polynuclear Organometallic Assemblies from a Simple
 Heteromultifunctional Ligand.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13670
_journal_page_last               13678
_journal_paper_doi               10.1021/jacs.5b08826
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C140 H156 F24 N16 O32 Rh8 S8'
_chemical_formula_weight         4110.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                98.627(3)
_cell_angle_beta                 99.679(4)
_cell_angle_gamma                113.369(2)
_cell_formula_units_Z            1
_cell_length_a                   13.862(2)
_cell_length_b                   17.169(3)
_cell_length_c                   20.376(5)
_cell_measurement_reflns_used    3985
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.63
_cell_measurement_theta_min      2.44
_cell_volume                     4260.6(14)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.989
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.1374
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27790
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.044
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions (three triflate anions) which could not be 
 restrained properly. Therefore, SQUEEZE algorithm was used 
 to omit them. 
;
_refine_diff_density_max         2.732
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         16532
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1856
_refine_ls_R_factor_gt           0.1083
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2912
_refine_ls_wR_factor_ref         0.3388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6719
_reflns_number_total             16532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08826_si_002.cif
_cod_data_source_block           3b-C2h
_cod_original_cell_volume        4260.4(14)
_cod_database_code               4129615
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2013-2
_shelx_res_checksum              35394
_shelx_hkl_checksum              88628