Synthesis and Characterization of PBP Pincer Iridium Complexes and Their Application in Alkane Transfer Dehydrogenation
Shih, Wei-Chun; Ozerov, Oleg V.; Organometallics 36 (2016) 228–; doi:10.1021/acs.organomet.6b00762

data_4089139
_publ_section_title
;
 Synthesis and Characterization of PBP Pincer Iridium Complexes and Their
 Application in Alkane Transfer Dehydrogenation
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              228
_journal_paper_doi               10.1021/acs.organomet.6b00762
_journal_volume                  36
_journal_year                    2016
_chemical_formula_moiety         'C26 H36 B Ir O2 P2'
_chemical_formula_sum            'C26 H36 B Ir O2 P2'
_chemical_formula_weight         645.50
_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             2016-01-22
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.593(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.512(7)
_cell_length_b                   15.357(10)
_cell_length_c                   15.506(10)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      29.087
_cell_measurement_theta_min      2.265
_cell_volume                     2640(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.950
_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  0.0618
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32325
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.580
_diffrn_reflns_theta_min         1.837
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.198
_exptl_absorpt_correction_T_max  0.4321
_exptl_absorpt_correction_T_min  0.2627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1398 before and 0.0783 after correction.
The Ratio of minimum to maximum transmission is 0.6080.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0296P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6056
_reflns_number_total             7040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00762_si_002.cif
_cod_data_source_block           6
_cod_original_cell_volume        2641(3)
_cod_database_code               4089139
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.423
_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.a Ternary CH refined with riding coordinates:
 C21(H21), C18(H18), C15(H15), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C13(H13), C12(H12), C11(H11)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              51563
_shelx_hkl_checksum              17350
_olex2_submission_special_instructions 'No special instructions were received'