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_4129610
_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            'C85 H146 F24 N20 O44 Pd4 Rh4 S8'
_chemical_formula_weight         3701.93
_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                70.251(2)
_cell_angle_beta                 70.323(2)
_cell_angle_gamma                81.884(2)
_cell_formula_units_Z            1
_cell_length_a                   15.1375(17)
_cell_length_b                   16.3127(18)
_cell_length_c                   16.5691(18)
_cell_measurement_reflns_used    6681
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.19
_cell_volume                     3624.2(7)
_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 0.981
_diffrn_measured_fraction_theta_max 0.982
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23458
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.327
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvents (one triflate anion, two methanol and 
 one water molecules) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         13987
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1371P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1958
_refine_ls_wR_factor_ref         0.2173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9179
_reflns_number_total             13987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08826_si_004.cif
_cod_data_source_block           10b
_cod_database_code               4129610
_shelx_estimated_absorpt_t_min   0.802
_shelx_estimated_absorpt_t_max   0.893
_shelxl_version_number           2013-2
_shelx_res_checksum              41705
_shelx_hkl_checksum              75859