Mechanistic studies on the addition of hydrogen to iridaepoxide complexes with subsequent elimination of water
Doyle, Lauren E.; Piers, Warren E.; Borau-Garcia, Javier; Sgro, Michael J.; Spasyuk, Denis M.; Chem. Sci. 7 (2016) 921–; doi:10.1039/C5SC03575A

data_1540437
_publ_section_title
;
 Mechanistic studies on the addition of hydrogen to iridaepoxide complexes
 with subsequent elimination of water
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              921
_journal_paper_doi               10.1039/C5SC03575A
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C29 H36 Br Ir O P2 S2, C7 H8 '
_chemical_formula_sum            'C36 H44 Br Ir O P2 S2'
_chemical_formula_weight         890.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-09-08 deposited with the CCDC.
2015-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.9590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5417(3)
_cell_length_b                   11.2071(2)
_cell_length_c                   22.7055(5)
_cell_measurement_reflns_used    9099
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.91
_cell_measurement_theta_min      3.23
_cell_volume                     3539.41(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'LinXTL v.  5.3.1'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         67.490
_diffrn_reflns_theta_min         3.235
_exptl_absorpt_coefficient_mu    10.789
_exptl_absorpt_correction_T_max  0.5230
_exptl_absorpt_correction_T_min  0.3974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6367
_refine_ls_number_restraints     387
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+2.3500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6097
_reflns_number_total             6367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03575a2.cif
_cod_data_source_block           1_Br
_cod_depositor_comments
'Adding full bibliography for 1540435--1540440.cif.'
_cod_database_code               1540437
_shelx_estimated_absorpt_t_min   0.221
_shelx_estimated_absorpt_t_max   0.221
_shelxl_version_number           2014/6
_shelx_res_checksum              66861