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_4517716
_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         'C26 H45 Ir O2 P2'
_chemical_formula_sum            'C26 H45 Ir O2 P2'
_chemical_formula_weight         643.76
_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
_audit_creation_date             2020-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6225(2)
_cell_length_b                   18.5843(4)
_cell_length_c                   17.0349(4)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.93
_cell_measurement_theta_min      3.06
_cell_volume                     2729.48(11)
_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      170.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0699
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25040
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.910
_diffrn_reflns_theta_min         3.062
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.385
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1916 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.6846.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.485
_refine_diff_density_min         -3.905
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5166
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0860P)^2^+14.7559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4367
_reflns_number_total             5166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00539_si_018.cif
_cod_data_source_block           mj19795_0m
_cod_depositor_comments
'Adding full bibliography for 4517711--4517721.cif.'
_cod_original_cell_volume        2729.49(11)
_cod_database_code               4517716
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.709
_shelx_estimated_absorpt_t_min   0.666
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C9A \\sim C2 \\sim C3 \\sim C4A \\sim C3A \\sim C2A \\sim C4 \\sim C9: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H5BC)=Sof(H5BD)=Sof(H8BC)=Sof(H8BD)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C2A)=
 Sof(H2A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H5AA)=Sof(H5AB)=
 Sof(H8AA)=Sof(H8AB)=Sof(C9)=Sof(H9A)=Sof(H9B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C15(H15), C18(H18), C21(H21), C24(H24), C2A(H2A), C3A(H3A)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5AA,H5AB), C5(H5BC,H5BD), C6(H6A,H6B), C7(H7A,H7B), C8(H8AA,
 H8AB), C8(H8BC,H8BD), C9(H9A,H9B), C4A(H4AA,H4AB), C9A(H9AA,H9AB)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              12966
_shelx_hkl_checksum              29010
_olex2_submission_special_instructions 'No special instructions were received'