A synthon for a 14-electron Ir(III) species: catalyst for highly selective beta-(Z) hydrosilylation of terminal alkynes
Manuel Iglesias; Maria Perez-Nicolas; Pablo J. Sanz Miguel; Victor Polo; Francisco J. Fernandez-Alvarez; Jesus J. Perez-Torrente; Luis A. Oro; Chem.Commun. 48 (2012) 9480–; doi:10.1039/c2cc34931k

data_7108330
_publ_section_title
;
 A synthon for a 14-electron Ir(III) species: catalyst for highly
 selective beta-(Z) hydrosilylation of terminal alkynes
;
_journal_name_full               Chem.Commun.
_journal_page_first              9480
_journal_paper_doi               10.1039/c2cc34931k
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C13 H20 I2 Ir N4 O2, B F4, C3 H6 O'
_chemical_formula_sum            'C16 H26 B F4 I2 Ir N4 O3'
_chemical_formula_weight         855.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-28T21:02:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5550(14)
_cell_length_b                   10.6594(8)
_cell_length_c                   11.3757(8)
_cell_measurement_reflns_used    6159
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.18
_cell_volume                     2371.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.96
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.034
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24968
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    8.291
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 2815 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6159
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.065
_reflns_number_gt                5962
_reflns_number_total             6159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34931k.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7108330
_refine_ls_number_parmeters      284