Half-sandwich Ir-based neutral organometallic macrocycles containing pyridine-4-thiolato ligands
Han, Ying-Feng; Lin, Yue-Jian; Jia, Wei-Guo; Jin, Guo-Xin; Dalton Transactions  (2009) 2077–2080; doi:10.1039/b900645c

data_7000792
_publ_section_title
;
 Half-sandwich Ir-based neutral organometallic macrocycles containing
 pyridine-4-thiolato ligands
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2077
_journal_page_last               2080
_journal_paper_doi               10.1039/b900645c
_journal_year                    2009
_chemical_formula_sum            'C45 H57 Cl3 Ir3 N3 S3'
_chemical_formula_weight         1419.07
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.877(5)
_cell_angle_beta                 85.029(6)
_cell_angle_gamma                88.798(5)
_cell_formula_units_Z            2
_cell_length_a                   8.838(3)
_cell_length_b                   17.675(7)
_cell_length_c                   18.572(7)
_cell_measurement_reflns_used    827
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.408
_cell_measurement_theta_min      2.506
_cell_volume                     2695.9(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.1092
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11192
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        11.00
_exptl_absorpt_coefficient_mu    7.682
_exptl_absorpt_correction_T_max  0.5138
_exptl_absorpt_correction_T_min  0.3920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.948
_refine_diff_density_min         -1.358
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         9285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                5578
_reflns_number_total             9285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b900645c.txt
_cod_data_source_block           f80405a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2695.9(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7000792