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_4129619
_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            'C195 H260 Cl32 F18 Ir12 N24 O40 S6'
_chemical_formula_weight         7555.43
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.131(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   37.603(5)
_cell_length_b                   21.407(3)
_cell_length_c                   38.008(5)
_cell_measurement_reflns_used    9138
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.63
_cell_measurement_theta_min      2.20
_cell_volume                     29391(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1232
_diffrn_reflns_av_sigmaI/netI    0.2056
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            146928
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         0.90
_diffrn_standards_decay_%        7.95
_exptl_absorpt_coefficient_mu    5.814
_exptl_absorpt_correction_T_max  0.4209
_exptl_absorpt_correction_T_min  0.3243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             14576
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (four triflate anions, two methanol, 
 twelve dichloromethane and eight water molecules) which 
 could not be restrained properly. Therefore, SQUEEZE 
 algorithm was used to omit them. 
;
_refine_diff_density_max         6.056
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1981
_refine_ls_number_reflns         51313
_refine_ls_number_restraints     1297
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.2182
_refine_ls_R_factor_gt           0.1135
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1844P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2877
_refine_ls_wR_factor_ref         0.3382
_reflns_number_gt                18229
_reflns_number_total             51313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b08826_si_003.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        29390(6)
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               4129619