Formation of Iridium(III) Allene Complexes via Isomerization of Internal Alkynes
Phadke, Neha; Findlater, Michael; Organometallics 33 (2014) 16–; doi:10.1021/om4010934

data_4082242
_publ_contact_author_email       michael.findlater@ttu.edu
_publ_contact_author_fax
;
;
_publ_contact_author_name        'Michael Findlater'
_publ_contact_author_phone
;
;
_publ_section_title
;
 Formation of Iridium(III) Allene Complexes via Isomerization of Internal
 Alkynes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              16
_journal_paper_doi               10.1021/om4010934
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C30 H53 Ir O2 P2'
_chemical_formula_sum            'C30 H53 Ir O2 P2'
_chemical_formula_weight         699.86
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2011-05-17
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled Feb 15 2011 20:38:53, GUI svn.r3494)
;
_cell_angle_alpha                92.411(2)
_cell_angle_beta                 91.896(2)
_cell_angle_gamma                109.056(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0369(3)
_cell_length_b                   10.6149(4)
_cell_length_c                   19.4286(7)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      2.28
_cell_volume                     1563.33(10)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22003
_diffrn_reflns_theta_full        66.95
_diffrn_reflns_theta_max         66.95
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'sealed tube'
_diffrn_source_current           40.0
_diffrn_source_power             1.6
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.403
_exptl_absorpt_correction_T_max  0.7092
_exptl_absorpt_correction_T_min  0.1004
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS-2008/1 (Bruker,2008) was used for absorption correction.
 R(int) was 0.0861 before and 0.0565 after correction.
 The Ratio of minimum to maximum transmission is 0.141567963903.
 The \l/2 correction factor is 0.0015
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.214
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5292
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+4.7683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                5047
_reflns_number_total             5292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4010934_si_002.cif
_cod_data_source_block           x1105002
_cod_database_code               4082242