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_4517720
_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 O2 P2 S'
_chemical_formula_sum            'C19 H31 Ir O2 P2 S'
_chemical_formula_weight         577.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 101.2420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.6785(5)
_cell_length_b                   8.07860(10)
_cell_length_c                   18.7571(3)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.935
_cell_measurement_theta_min      5.268
_cell_volume                     4410.93(12)
_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 0.995
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23079
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.923
_diffrn_reflns_theta_min         5.266
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.653
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1455 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.7525. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4175
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+7.8788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0365
_refine_ls_wR_factor_ref         0.0370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3999
_reflns_number_total             4175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00539_si_022.cif
_cod_data_source_block           mj19302_0m
_cod_depositor_comments
'Adding full bibliography for 4517711--4517721.cif.'
_cod_original_cell_volume        4410.92(12)
_cod_database_code               4517720
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.644
_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
 S1A-P1
 2.1 with sigma of 0.02
3. Rigid bond restraints
 P2, S1, P1, O2, S1, C7, O2, C3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Uiso/Uaniso restraints and constraints
P2 \\sim S1: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.001
O2A \\sim S1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O2 \\sim S1A \\sim O2A \\sim S1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C2 \\sim C2A \\sim C7A \\sim C6A \\sim C5A \\sim C4A \\sim C3A \\sim C3 \\sim
C7 \\sim C6 \\sim C5 \\sim C4 \\sim S1A \\sim O2 \\sim O2A \\sim S1: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2A) \\sim Ueq, Uanis(S1A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Sof(S1A)=Sof(O2A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C4A)=Sof(H4A)=
 Sof(C7A)=Sof(C3A)=Sof(C2A)=1-FVAR(1)
 Sof(S1)=Sof(O2)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(H6)=Sof(C7)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C14(H14), C17(H17)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C5A(H5A), C6A(H6A), C4A(H4A)
6.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)
;
_shelx_res_checksum              8659
_shelx_hkl_checksum              12882
_olex2_submission_special_instructions 'No special instructions were received'