Stepwise Reactions of Acetylenes with Iridium Thiocarbonyl Complexes To Produce Isolable Iridacyclobutadienes and Conversion of These to either Cyclopentadienyliridium or Tethered Iridabenzene Complexes
Clark, George R.; Lu, Guo-Liang; Roper, Warren R.; Wright, L. James; Organometallics 26 (2007) 2167–; doi:10.1021/om061066r

data_4072825
_publ_section_title
;
 Stepwise Reactions of Acetylenes with Iridium Thiocarbonyl Complexes To
 Produce Isolable Iridacyclobutadienes and Conversion of These to either
 Cyclopentadienyliridium or Tethered Iridabenzene Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2167
_journal_paper_doi               10.1021/om061066r
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C53 H42 Cl Ir P2 S, C H2 Cl2, 3(C2 H6 O)'
_chemical_formula_sum            'C60 H62 Cl3 Ir O3 P2 S'
_chemical_formula_weight         1223.65
_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                85.507(1)
_cell_angle_beta                 83.165(1)
_cell_angle_gamma                80.417(1)
_cell_formula_units_Z            2
_cell_length_a                   10.6941(1)
_cell_length_b                   12.0101(1)
_cell_length_c                   19.9108(0)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.06
_cell_volume                     2499.20(3)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SADABS (Sheldrick, 1997)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      83(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'Area detector \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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            24876
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.986
_exptl_absorpt_correction_T_max  0.66035
_exptl_absorpt_correction_T_min  0.46199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1997'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details          ' ?'
_refine_diff_density_max         3.775
_refine_diff_density_min         -2.090
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0772
_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^)+(0.0729P)^2^+27.6858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1894
_refine_ls_wR_factor_ref         0.1930
_reflns_number_gt                8026
_reflns_number_total             8816
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om061066rsi20070208_115402.cif
_cod_data_source_block           lu480e
_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.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (17
times).

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (95
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (13
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (175 times).

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               4072825