Site-Selective Alkyl Dehydrogenation of a Coordinated Acylphosphine Ligand
Whittemore, Sean M.; Yoder, Ryan J.; Stambuli, James P.; Organometallics 31 (2012) 6124–; doi:10.1021/om300471h

data_4079088
_publ_section_title
;
 Site-Selective Alkyl Dehydrogenation of a Coordinated Acylphosphine
 Ligand
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6124
_journal_paper_doi               10.1021/om300471h
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H57 Cl2 Ir2 O P, 2(P F6), 2(C H2 Cl2)'
_chemical_formula_sum            'C35 H61 Cl6 F12 Ir2 O P3'
_chemical_formula_weight         1415.85
_chemical_name_common            'Stambuli 1864'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-11-30T11:44:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.404(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8532(3)
_cell_length_b                   38.7135(7)
_cell_length_c                   17.0068(3)
_cell_measurement_reflns_used    23022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     9903.8(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.215375E-1
_diffrn_orient_matrix_UB_12      0.155824E-1
_diffrn_orient_matrix_UB_13      0.49185E-1
_diffrn_orient_matrix_UB_21      0.118092E-1
_diffrn_orient_matrix_UB_22      0.185453E-1
_diffrn_orient_matrix_UB_23      -0.360975E-1
_diffrn_orient_matrix_UB_31      -0.617651E-1
_diffrn_orient_matrix_UB_32      0.89794E-2
_diffrn_orient_matrix_UB_33      -0.108005E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            187306
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.37
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.864
_exptl_absorpt_correction_T_max  0.626
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5504
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.447
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         22695
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+26.1103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                16966
_reflns_number_total             22695
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om300471h_si_002.cif
_cod_data_source_block           Stambuli1864
_cod_depositor_comments
;

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C70 H122 Cl12 F24 Ir4 O2 P6'
_cod_original_formula_weight         2831.7
_cod_original_formula_moiety
'C66 H114 Cl4 Ir4 O2 P2, 4(P F6), 4 (C H2 Cl2)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      ' P 21/c'
_cod_database_code               4079088