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_4129609
_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            'C77 H114 F24 Ir4 N20 O38 Pd4 S8'
_chemical_formula_weight         3834.76
_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                70.478(2)
_cell_angle_beta                 70.163(2)
_cell_angle_gamma                82.134(2)
_cell_formula_units_Z            1
_cell_length_a                   15.226(2)
_cell_length_b                   16.217(2)
_cell_length_c                   16.576(3)
_cell_measurement_reflns_used    4576
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.43
_cell_volume                     3627.5(9)
_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 0.984
_diffrn_measured_fraction_theta_max 0.985
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.1039
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23501
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.923
_exptl_absorpt_coefficient_mu    4.353
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 triflate anion which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit it. 
;
_refine_diff_density_max         1.686
_refine_diff_density_min         -2.689
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         14045
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0576
_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^)+(0.1061P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8070
_reflns_number_total             14045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08826_si_004.cif
_cod_data_source_block           10a
_cod_original_cell_volume        3627.4(9)
_cod_database_code               4129609
_shelx_estimated_absorpt_t_min   0.543
_shelx_estimated_absorpt_t_max   0.918
_shelxl_version_number           2013-2
_shelx_res_checksum              79503
_shelx_hkl_checksum              32904