Elucidation of Heterocumulene Activation by a Nucleophilic-at-Metal Iridium(I) Carbene
Whited, Matthew T.; Grubbs, Robert H.; Organometallics 28 (2009) 161–; doi:10.1021/om8009766

data_4068601
_publ_section_title
;
 Elucidation of Heterocumulene Activation by a Nucleophilic-at-Metal
 Iridium(I) Carbene
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              161
_journal_paper_doi               10.1021/om8009766
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C27 H40 Ir N P2 S'
_chemical_formula_weight         664.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 113.660(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8273(10)
_cell_length_b                   13.4512(9)
_cell_length_c                   16.6229(12)
_cell_measurement_reflns_used    9694
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      39.12
_cell_measurement_theta_min      2.21
_cell_volume                     2831.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_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  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            110694
_diffrn_reflns_theta_full        38.17
_diffrn_reflns_theta_max         39.58
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    4.916
_exptl_absorpt_correction_T_max  0.582
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         25.955
_refine_diff_density_min         -15.160
_refine_diff_density_rms         0.507
_refine_ls_abs_structure_details 'Flack (1983), 12584 Friedel pairs'
_refine_ls_abs_structure_Flack   0.065(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         29430
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.1060
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1330P)^2^+94.3564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2813
_refine_ls_wR_factor_ref         0.2971
_reflns_number_gt                23242
_reflns_number_total             29430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8009766_si_002.cif
_cod_data_source_block           mtw81abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pn
_cod_database_code               4068601