N-Bridged Pincer Iridium Complexes for Highly Efficient Alkane Dehydrogenation and the Relevant Linker Effects
Zhang, Xin; Wu, Song-Bai; Leng, Xuebing; Chung, Lung Wa; Liu, Guixia; Huang, Zheng; ACS Catalysis  (2020) 6475–6487; doi:10.1021/acscatal.0c00539

data_4517721
_publ_section_title
;
 N-Bridged Pincer Iridium Complexes for Highly Efficient Alkane
 Dehydrogenation and the Relevant Linker Effects
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              6475
_journal_page_last               6487
_journal_paper_doi               10.1021/acscatal.0c00539
_journal_year                    2020
_chemical_formula_moiety         'C19 H31 Ir O3 P2'
_chemical_formula_sum            'C19 H31 Ir O3 P2'
_chemical_formula_weight         561.58
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                108.3700(10)
_cell_angle_beta                 97.8940(10)
_cell_angle_gamma                91.0830(10)
_cell_formula_units_Z            6
_cell_length_a                   14.2131(3)
_cell_length_b                   14.3576(3)
_cell_length_c                   17.1807(4)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.919
_cell_measurement_theta_min      3.895
_cell_volume                     3288.59(13)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      169.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47601
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.965
_diffrn_reflns_theta_min         2.828
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.154
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1435 before and 0.0858 after correction. The Ratio of minimum to maximum transmission is 0.5302. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.194
_refine_diff_density_min         -3.808
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         12494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+7.0898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11481
_reflns_number_total             12494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00539_si_002.cif
_cod_data_source_block           mjl18646_0m
_cod_depositor_comments
'Adding full bibliography for 4517711--4517721.cif.'
_cod_original_cell_volume        3288.58(13)
_cod_database_code               4517721
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.406
_shelx_estimated_absorpt_t_min   0.290
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C14(H14), C17(H17), C8A(H8A), C11A(H11A), C14A(H14A),
 C17A(H17A), C8B(H8B), C11B(H11B), C14B(H14B), C17B(H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C4A(H4A), C5A(H5A), C6A(H6A), C4B(H4B), C5B(H5B),
 C6B(H6B)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,
 H19B,H19C), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C12A(H12D,H12E,H12F),
 C13A(H13D,H13E,H13F), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F), C18A(H18D,
 H18E,H18F), C19A(H19D,H19E,H19F), C9B(H9BA,H9BB,H9BC), C10B(H10G,H10H,H10I),
 C12B(H12G,H12H,H12I), C13B(H13G,H13H,H13I), C15B(H15G,H15H,H15I), C16B(H16G,
 H16H,H16I), C18B(H18G,H18H,H18I), C19B(H19G,H19H,H19I)
;
_shelx_res_checksum              66375
_shelx_hkl_checksum              83296
_olex2_submission_special_instructions 'No special instructions were received'