Hydrogen and oxygen activation by an iridium precursor containing the 4,5-bis(diphenylthiophosphinoyl)-1,2,3-triazole ligand
Zúñiga-Villarreal, Noé; Hernández-Juárez, Martín; Toscano, Ruben Alfredo; Cortes-Guzman, Fernando; RSC Adv.  (2015) –; doi:10.1039/C5RA07698F

data_7220918
_publ_section_title
;
 Hydrogen and oxygen activation by an iridium precursor containing the
 4,5-bis(diphenylthiophosphinoyl)-1,2,3-triazole ligand
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA07698F
_journal_year                    2015
_chemical_formula_moiety         'C42 H48 Ir N3 P2 S2, C7 H8'
_chemical_formula_sum            'C49 H56 Ir N3 P2 S2'
_chemical_formula_weight         1005.22
_chemical_name_systematic        '[Ir(\k2-S,N-(4,5-(P(S)Ph2)2Tz))(coe)2] '
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-04-24 deposited with the CCDC.
2015-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.251(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.944(3)
_cell_length_b                   17.317(3)
_cell_length_c                   20.834(4)
_cell_measurement_reflns_used    1739
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      2.34
_cell_volume                     4505.5(16)
_computing_cell_refinement       'APEX2 v2012.10.0(Bruker, 2012)'
_computing_data_collection       'APEX2 v2012.10.0(Bruker, 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker, 2012)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker Smart Apex CCD diffractometer 01-670-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2242
_diffrn_reflns_av_unetI/netI     0.2378
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22307
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.552
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.164
_exptl_absorpt_correction_T_max  0.8785
_exptl_absorpt_correction_T_min  0.3612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.042
_refine_diff_density_max         3.345
_refine_diff_density_min         -3.025
_refine_diff_density_rms         0.242
_refine_ls_extinction_coef       0.00072(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8244
_refine_ls_number_restraints     382
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1906
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0954P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3838
_reflns_number_total             8244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra07698f2.cif
_cod_data_source_block           Compound_1
_cod_database_code               7220918
_shelx_estimated_absorpt_t_min   0.361
_shelx_estimated_absorpt_t_max   0.879
_shelxl_version_number           2013-4
_shelx_res_checksum              59796