Stepwise Formation of Tetra- and Hexanuclear Iridium and Rhodium Complexes Containing Oxalato Ligands
Han, Ying-Feng; Lin, Yue-Jian; Jia, Wei-Guo; Weng, Lin-Hong; Jin, Guo-Xin; Organometallics 26 (2007) 5848–; doi:10.1021/om700691u

data_4073864
_publ_section_title
;
 Stepwise Formation of Tetra- and Hexanuclear Iridium and Rhodium
 Complexes Containing Oxalato Ligands
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5848
_journal_paper_doi               10.1021/om700691u
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C70 H84 Cl4 F12 Ir4 N4 O22 S4'
_chemical_formula_weight         2600.25
_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                95.394(12)
_cell_angle_beta                 111.274(10)
_cell_angle_gamma                116.316(9)
_cell_formula_units_Z            1
_cell_length_a                   12.685(10)
_cell_length_b                   14.250(11)
_cell_length_c                   15.672(12)
_cell_measurement_reflns_used    840
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.360
_cell_measurement_theta_min      2.897
_cell_volume                     2253(3)
_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 0.899
_diffrn_measured_fraction_theta_max 0.899
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9948
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        5.85
_exptl_absorpt_coefficient_mu    6.191
_exptl_absorpt_correction_T_max  0.5764
_exptl_absorpt_correction_T_min  0.3707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.826
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.826
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                5088
_reflns_number_total             9069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700691u-file002.cif
_cod_data_source_block           f70327c
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073864