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_1540436
_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 Ir O2 P2 S2, 0.5(C7 H8)'
_chemical_formula_sum            'C32.5 H40 Ir O2 P2 S2'
_chemical_formula_weight         780.90
_chemical_name_systematic
;
 ?
;
_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   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-09-08 deposited with the CCDC.
2015-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                105.409(2)
_cell_angle_beta                 103.594(2)
_cell_angle_gamma                93.729(2)
_cell_formula_units_Z            4
_cell_length_a                   12.8155(7)
_cell_length_b                   14.1374(8)
_cell_length_c                   19.4358(11)
_cell_measurement_temperature    173(2)
_cell_volume                     3269.0(3)
_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.  5.3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0585
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_laue_measured_fraction_full 0.969
_diffrn_reflns_laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40418
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         67.493
_diffrn_reflns_theta_min         2.444
_exptl_absorpt_coefficient_mu    10.236
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.780
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         11415
_refine_ls_number_restraints     729
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+3.0386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10577
_reflns_number_total             11415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03575a2.cif
_cod_data_source_block           1_OH
_cod_depositor_comments
;
Adding full bibliography for 1540435--1540440.cif.

2019-02-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C65 H80 Ir2 O4 P4 S4'
_cod_original_formula_weight         1561.81
_cod_original_formula_moiety         '2(C29 H36 Ir O2 P2 S2), C7 H8'
_cod_original_formula_units_Z            2
_cod_database_code               1540436
_shelx_estimated_absorpt_t_min   0.184
_shelx_estimated_absorpt_t_max   0.399
_shelxl_version_number           2013-4
_shelx_res_checksum              85841