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_4517719
_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         'C22 H36 Ir N O2 P2'
_chemical_formula_sum            'C22 H36 Ir N O2 P2'
_chemical_formula_weight         600.66
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.6750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6088(2)
_cell_length_b                   11.1953(2)
_cell_length_c                   15.5695(3)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      56.965
_cell_measurement_theta_min      5.842
_cell_volume                     2331.03(7)
_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      170.01
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22542
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         56.937
_diffrn_reflns_theta_min         6.781
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.626
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.4777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1068 before and 0.0470 after correction. The Ratio of minimum to maximum transmission is 0.6359. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0108P)^2^+2.7611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4553
_reflns_number_total             4588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00539_si_009.cif
_cod_data_source_block           mjl18149_0m
_cod_depositor_comments
'Adding full bibliography for 4517711--4517721.cif.'
_cod_database_code               4517719
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.479
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C16(H16), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C)
;
_shelx_res_checksum              64592
_shelx_hkl_checksum              31362
_olex2_submission_special_instructions 'No special instructions were received'