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_1546816
_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         'C48 H68 Cl Ir N4 Si2, 3(C H2 Cl2)'
_chemical_formula_sum            'C51 H74 Cl7 Ir N4 Si2'
_chemical_formula_weight         1239.67
_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   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                83.648(3)
_cell_angle_beta                 87.998(3)
_cell_angle_gamma                76.732(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0773(4)
_cell_length_b                   13.0942(4)
_cell_length_c                   22.7288(8)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.2530
_cell_measurement_theta_min      3.8860
_cell_volume                     2901.04(18)
_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 0.805
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.805
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24460
_diffrn_reflns_point_group_measured_fraction_full 0.805
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        90.000
_diffrn_reflns_theta_max         69.423
_diffrn_reflns_theta_min         3.487
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.090
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.217
_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            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.088
_refine_diff_density_max         2.089
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         10657
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+2.0883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9468
_reflns_number_total             10657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04832g2.cif
_cod_data_source_block           4_CH2Cl2_3
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2020-12-11
;
_cod_database_code               1546816
_shelxl_version_number           2014-3
_shelx_res_checksum              9662