Facile cyclometallation of a mesitylsilylene: synthesis and preliminary catalytic activity of iridium(III) and iridium(V) iridasilacyclopentenes
Cabeza, Javier A.; García-Álvarez, Pablo; González-Álvarez, Laura; Chemical Communications 53 (2017) 10275–10278; doi:10.1039/C7CC04832G

data_1546817
_publ_section_title
;
 Facile cyclometallation of a mesitylsilylene: synthesis and preliminary
 catalytic activity of iridium(III) and iridium(V) iridasilacyclopentenes
;
_journal_issue                   74
_journal_name_full               'Chemical Communications'
_journal_page_first              10275
_journal_page_last               10278
_journal_paper_doi               10.1039/C7CC04832G
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C32 H46 Cl Ir N2 Si, 0.5(C7 H8)'
_chemical_formula_sum            'C35.5 H50 Cl Ir N2 Si'
_chemical_formula_weight         760.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-06-19 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.903(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2028(13)
_cell_length_b                   9.0196(3)
_cell_length_c                   20.2302(12)
_cell_measurement_reflns_used    6458
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.1700
_cell_measurement_theta_min      4.3800
_cell_volume                     3343.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2016)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.808
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.808
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16841
_diffrn_reflns_point_group_measured_fraction_full 0.808
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        90.000
_diffrn_reflns_theta_max         69.694
_diffrn_reflns_theta_min         4.388
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.994
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pale-orange
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       prism
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.435
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6180
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.8300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5022
_reflns_number_total             6180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04832g2.cif
_cod_data_source_block           3_toluene_05
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2020-12-11
;
_cod_original_formula_sum        'C35.50 H50 Cl Ir N2 Si'
_cod_database_code               1546817
_shelxl_version_number           2014-3
_shelx_res_checksum              95534