Syntheses and Reactions of Half-Sandwich Iridium, Rhodium, and Ruthenium Metallacycles Containing 4-Pyridyl Dithioether Ligands
Jia, Ai-Quan; Han, Ying-Feng; Lin, Yue-Jian; Jin, Guo-Xin; Organometallics 29 (2010) 232–240; doi:10.1021/om900921g

data_4067400
_publ_section_title
;
 Syntheses and Reactions of Half-Sandwich Iridium, Rhodium, and Ruthenium
 Metallacycles Containing 4-Pyridyl Dithioether Ligands
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              232
_journal_page_last               240
_journal_paper_doi               10.1021/om900921g
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C64 H67 Cl3 F9 Ir3 N2 O13 S5'
_chemical_formula_weight         2086.45
_chemical_name_systematic        ?
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.803(6)
_cell_length_b                   42.770(17)
_cell_length_c                   10.751(4)
_cell_measurement_reflns_used    952
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.012
_cell_measurement_theta_min      2.372
_cell_volume                     7267(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.1421
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            34110
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        5.23
_exptl_absorpt_coefficient_mu    5.818
_exptl_absorpt_correction_T_max  0.5938
_exptl_absorpt_correction_T_min  0.4757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         15209
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                8871
_reflns_number_total             15209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900921g_si_001.cif
_cod_data_source_block           4a(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4067400