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_4517711
_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         'C23 H42 Cl Ir N P2 S'
_chemical_formula_sum            'C23 H42 Cl Ir N P2 S'
_chemical_formula_weight         654.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2672(2)
_cell_length_b                   15.0400(3)
_cell_length_c                   28.7115(6)
_cell_measurement_reflns_used    9232
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      60.607
_cell_measurement_theta_min      4.125
_cell_volume                     5297.23(18)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0656
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            49974
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.997
_diffrn_reflns_theta_min         4.124
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.649
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.4985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1878 before and 0.0897 after correction. The Ratio of minimum to maximum transmission is 0.6630. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5038
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+8.5958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4421
_reflns_number_total             5038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00539_si_016.cif
_cod_data_source_block           mjl18048_0m
_cod_depositor_comments
'Adding full bibliography for 4517711--4517721.cif.'
_cod_database_code               4517711
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.781
_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. Restrained distances
 N1-C7
 1.53 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
N1 \\sim C6 \\sim C7: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
N4 \\sim C7A \\sim C2 \\sim P1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Cl1 \\sim Cl1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Fixed Sof: S1(0.66667) N1(0.66667) C7(0.66667) H7A(0.66667) H7B(0.66667)
 H7C(0.66667) S2(0.33333) C7A(0.33333) H7AA(0.33333) H7AB(0.33333)
 H7AC(0.33333) N4(0.33333)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C7A(H7AA,H7AB,H7AC)
;
_shelx_res_checksum              87294
_shelx_hkl_checksum              91945
_olex2_submission_special_instructions 'No special instructions were received'