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_7220921
_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         'C62 H52 Ir N3 P4 S2, 0.5(C H Cl3)'
_chemical_formula_sum            'C62.5 H52.5 Cl1.5 Ir N3 P4 S2'
_chemical_formula_weight         1278.95
_chemical_name_systematic        '[Ir(\k2-S,N-(4,5-(P(S)Ph2)2Tz))(PPh3)2(H)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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-04-24 deposited with the CCDC.
2015-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0119(10)
_cell_length_b                   23.8515(16)
_cell_length_c                   17.8353(12)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.19
_cell_volume                     5880.7(7)
_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, 2014/1)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39841
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.063
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.560
_exptl_absorpt_correction_T_max  0.7102
_exptl_absorpt_correction_T_min  0.5828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       prism
_exptl_crystal_F_000             2572
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.142
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         13418
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0570P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10110
_reflns_number_total             13418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra07698f2.cif
_cod_data_source_block           Compound_5a
_cod_original_formula_sum        'C62.50 H52.50 Cl1.50 Ir N3 P4 S2'
_cod_database_code               7220921
_shelx_estimated_absorpt_t_min   0.586
_shelx_estimated_absorpt_t_max   0.713
_shelxl_version_number           2014-1
_shelx_res_checksum              44386