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_7132417
_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         'C19 H18 Cl Ir N4 O3'
_chemical_formula_sum            'C19 H18 Cl Ir N4 O3'
_chemical_formula_weight         578.02
_chemical_name_systematic        IrtpyMeester
_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                 100.974(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1369(5)
_cell_length_b                   12.5428(4)
_cell_length_c                   22.7604(7)
_cell_measurement_reflns_used    7594
_cell_measurement_temperature    143
_cell_measurement_theta_max      28.9880
_cell_measurement_theta_min      2.1780
_cell_volume                     3962.0(2)
_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 0.872
_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     48.00  74.00   0.50  100.00    --  -12.50  46.00-180.00   52
  2  \w   -101.00  76.00   0.50  100.00    --  -12.50  46.00 -90.00  354
  3  \w    -54.00 -28.00   0.50  100.00    --  -12.50  28.00  30.00   52
  4  \w     26.00  51.00   0.50  100.00    --  -12.50  28.00  30.00   50
  5  \w    -87.00   3.00   0.50  100.00    --  -12.50  46.00-180.00  180
;
_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      -0.0483762000
_diffrn_orient_matrix_UB_12      0.0154124000
_diffrn_orient_matrix_UB_13      -0.0003070000
_diffrn_orient_matrix_UB_21      -0.0078898000
_diffrn_orient_matrix_UB_22      0.0050526000
_diffrn_orient_matrix_UB_23      -0.0315946000
_diffrn_orient_matrix_UB_31      -0.0145217000
_diffrn_orient_matrix_UB_32      -0.0541590000
_diffrn_orient_matrix_UB_33      -0.0030410000
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16778
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.590
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45733
_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            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+4.8472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3894
_reflns_number_total             4851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05285k2.cif
_cod_data_source_block           230130_irtpyester
_cod_database_code               7132417
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'Ir1 C15 H11 N3 Cl1 O2'
_chemical_oxdiff_usercomment     small_Orange_ANMeOHEt2O
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.644
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C16(H16), C11(H11), C13(H13), C17(H17), C18(H18), C12(H12), C7(H7),
 C6(H6), C8(H8), C19(H19), C5(H5)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 68 electrons were 
found in a volume of 288\%A^3 in 1 void. 
This is consistent with the presence of 
0.4[CH4O] per formula unit 
which account for 72.0 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93947
_shelx_hkl_checksum              11945
_shelx_fab_checksum              31480
_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 2.012
_oxdiff_exptl_absorpt_empirical_full_min 0.689