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_4067397
_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            'C124 H148 Cl8 F12 Ir4 N4 O24 S8'
_chemical_formula_weight         3615.34
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.984(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.7100(19)
_cell_length_b                   26.661(3)
_cell_length_c                   14.8575(15)
_cell_measurement_reflns_used    4320
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.16
_cell_measurement_theta_min      2.31
_cell_volume                     7410.2(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.1205
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40561
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        3.67
_exptl_absorpt_coefficient_mu    3.916
_exptl_absorpt_correction_T_max  0.7712
_exptl_absorpt_correction_T_min  0.4410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            translucent
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.576
_refine_diff_density_min         -1.898
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         15132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1573
_reflns_number_gt                7527
_reflns_number_total             15132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900921g_si_001.cif
_cod_data_source_block           2a(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        7410.1(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4067397