Storing electrons from H<sub>2</sub> for transfer to CO<sub>2</sub>, all at room temperature.
Shimauchi, Daiki; Yatabe, Takeshi; Ikesue, Yuka; Kajiwara, Yuu; Koide, Taro; Ando, Tatsuya; Yoon, Ki-Seok; Nakai, Hidetaka; Ogo, Seiji; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc05285k

data_7132416
_publ_section_title
;
 Storing electrons from H<sub>2</sub> for transfer to CO<sub>2</sub>, all
 at room temperature.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc05285k
_journal_year                    2023
_chemical_formula_moiety         'C17 H14 Cl Ir N4, F6 P, C2 H3 N'
_chemical_formula_sum            'C19 H17 Cl F6 Ir N5 P'
_chemical_formula_weight         687.99
_chemical_name_systematic        Ir2tpy2Cl2AN2PF6
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-10-19 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.818(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0860(12)
_cell_length_b                   12.9848(9)
_cell_length_c                   25.954(3)
_cell_measurement_reflns_used    3086
_cell_measurement_temperature    143
_cell_measurement_theta_max      27.0930
_cell_measurement_theta_min      3.1360
_cell_volume                     4358.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      143
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00   2.00   0.50  100.00    --    5.00  28.00 -60.00   54
  2  \w     -7.00  29.00   0.50  100.00    --  -12.30  46.00   0.00   72
  3  \w    -74.00  74.00   0.50  100.00    --  -12.30  55.00  60.00  296
  4  \w   -100.00 -17.00   0.50  100.00    --  -12.30  46.00   0.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0443020000
_diffrn_orient_matrix_UB_12      0.0320796000
_diffrn_orient_matrix_UB_13      0.0040667000
_diffrn_orient_matrix_UB_21      0.0306463000
_diffrn_orient_matrix_UB_22      -0.0426288000
_diffrn_orient_matrix_UB_23      0.0100970000
_diffrn_orient_matrix_UB_31      0.0101875000
_diffrn_orient_matrix_UB_32      -0.0117837000
_diffrn_orient_matrix_UB_33      -0.0254250000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            15271
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.589
_diffrn_reflns_theta_min         2.588
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.097
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.413
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0304P)^2^+53.8470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3671
_reflns_number_total             5196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05285k2.cif
_cod_data_source_block           230131_irtpyclanpf6
_cod_original_cell_volume        4357.9(7)
_cod_database_code               7132416
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'Ir2 C30 H22 N6 Cl2 P2 F12'
_chemical_oxdiff_usercomment     AN_Et2O
_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 Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C4(H4), C15(H15), C7(H7), C3(H3), C2(H2), C14(H14), C9(H9),
 C12(H12), C13(H13)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              75910
_shelx_hkl_checksum              27623
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.791
_oxdiff_exptl_absorpt_empirical_full_min 0.777