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_4129623
_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            'C122 H160 Cl4 F24 N16 O36 Rh8 S8'
_chemical_formula_weight         4104.21
_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                64.831(2)
_cell_angle_beta                 69.578(2)
_cell_angle_gamma                89.812(2)
_cell_formula_units_Z            1
_cell_length_a                   15.2242(18)
_cell_length_b                   16.905(2)
_cell_length_c                   18.103(2)
_cell_measurement_reflns_used    4675
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.86
_cell_measurement_theta_min      2.28
_cell_volume                     3893.4(8)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25269
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.804
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       sheet
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (half of one triflate anion and two 
 methanol molecules) which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit them. 
;
_refine_diff_density_max         3.027
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         15092
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1545
_refine_ls_R_factor_gt           0.0959
_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          0.2660
_refine_ls_wR_factor_ref         0.3178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8121
_reflns_number_total             15092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08826_si_006.cif
_cod_data_source_block           2b-C2h
_cod_original_cell_volume        3893.6(8)
_cod_database_code               4129623
_shelx_estimated_absorpt_t_min   0.769
_shelx_estimated_absorpt_t_max   0.860
_shelxl_version_number           2013-2
_shelx_res_checksum              65024
_shelx_hkl_checksum              34336