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_4072829
_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_sum            'C59.5 H52.5 Cl Ir O6 P2 S'
_chemical_formula_weight         1185.17
_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                 100.255(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0065(4)
_cell_length_b                   19.2784(6)
_cell_length_c                   22.4702(8)
_cell_measurement_reflns_used    7323
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      1.72
_cell_volume                     5118.0(3)
_computing_cell_refinement       'Siemens SMART (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SAINT (Siemens, 1995)'
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material  'Siemens SMART (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1990)'
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29039
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.817
_exptl_absorpt_correction_T_max  0.6027
_exptl_absorpt_correction_T_min  0.4476
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 1997'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2390
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+10.4179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0567
_reflns_number_gt                8648
_reflns_number_total             9672
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om061066rsi20070208_115402.cif
_cod_data_source_block           lu488
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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 (16
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 (109
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 (31
time).

'_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 (172 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C59.50 H52.50 Cl Ir O6 P2 S'
_cod_database_code               4072829