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_4517718
_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         'C20 H37 Ir O2 P2 S0.99'
_chemical_formula_sum            'C20 H37 Ir O2 P2 S0.99'
_chemical_formula_weight         595.37
_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                 92.063(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.059(13)
_cell_length_b                   8.033(5)
_cell_length_c                   16.181(11)
_cell_measurement_reflns_used    1915
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.81
_cell_measurement_theta_min      2.52
_cell_volume                     2476(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_av_unetI/netI     0.1101
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16192
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         1.069
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.616
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1053 before and 0.0668 after correction. The Ratio of minimum to maximum transmission is 0.6667. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_description       plate
_exptl_crystal_F_000             1183
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         8.069
_refine_diff_density_min         -1.733
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4342
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.1095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+65.4625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2384
_refine_ls_wR_factor_ref         0.2608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2844
_reflns_number_total             4342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00539_si_020.cif
_cod_data_source_block           dm19029
_cod_depositor_comments
'Adding full bibliography for 4517711--4517721.cif.'
_cod_database_code               4517718
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.604
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.930(8)
 0.070(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 S1-C20 = S1-C19 = S1A-C19A = S1A-C20A
 1.85 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
S1A \\sim S1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S1 \\sim C19 \\sim C20: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
S1A \\sim C20A \\sim C19A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C19A) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C19)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C19A)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C16(H16)
6.b Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), 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), C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              75726
_shelx_hkl_checksum              48991
_olex2_submission_special_instructions 'No special instructions were received'