Visible light-driven CO2 reduction with a Ru polypyridyl complex bearing an N-heterocyclic carbene moiety
Watanabe, Taito; Saga, Yutaka; Kosugi, Kento; Iwami, Hikaru; Kondo, Mio; Masaoka, Shigeyuki; Chemical Communications  (2022) –; doi:10.1039/D2CC00657J

data_7129880
_publ_section_title
;
 Visible light-driven CO2 reduction with a Ru polypyridyl complex bearing
 an N-heterocyclic carbene moiety
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00657J
_journal_year                    2022
_chemical_formula_moiety         'C27 H25 N7 Ru, 2(C24 H20 B)'
_chemical_formula_sum            'C75 H65 B2 N7 Ru'
_chemical_formula_weight         1187.03
_chemical_name_systematic        RuC(BPh4)2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-02-17 deposited with the CCDC.	2022-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   40.5571(6)
_cell_length_b                   24.8192(4)
_cell_length_c                   24.1742(5)
_cell_measurement_reflns_used    36594
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.3850
_cell_measurement_theta_min      1.8860
_cell_volume                     24333.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.882
_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     -8.00  86.00   0.50   90.00    --   11.89  57.00 -90.00  188
  2  \w    -20.00  92.00   0.50   90.00    --   11.89  19.00-164.00  224
  3  \w    -10.00  19.00   0.50   90.00    --  -11.66 -99.00 -60.00   58
  4  \w    -24.00   4.00   0.50   90.00    --  -11.66 -99.00-180.00   56
  5  \w    -77.00  11.00   0.50   90.00    --  -11.66 -38.00 -90.00  176
  6  \w    -65.00  38.00   0.50   90.00    --   11.89 -19.00  27.00  206
  7  \w    -25.00   7.00   0.50   90.00    --  -11.66 -99.00 150.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0016318000
_diffrn_orient_matrix_UB_12      -0.0066656000
_diffrn_orient_matrix_UB_13      0.0284099000
_diffrn_orient_matrix_UB_21      -0.0041740000
_diffrn_orient_matrix_UB_22      -0.0271285500
_diffrn_orient_matrix_UB_23      -0.0060522500
_diffrn_orient_matrix_UB_31      0.0168926000
_diffrn_orient_matrix_UB_32      -0.0060368000
_diffrn_orient_matrix_UB_33      -0.0042565000
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            86451
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.283
_diffrn_reflns_theta_min         1.911
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             9888
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.069
_refine_diff_density_max         2.303
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(3)
_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     768
_refine_ls_number_reflns         16620
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0790P)^2^+25.8171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                14177
_reflns_number_total             16620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00657j2.cif
_cod_data_source_block           wt-53-bph4
_cod_database_code               7129880
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Ru C H N B O'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(3)
 0.11(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C105(H105), C117(H117), C106(H106), C118(H118), C220(H220), C109(H109),
 C104(H104), C10(H10), C115(H115), C13(H13), C3(H3), C203(H203), C214(H214),
 C212(H212), C14(H14), C4(H4), C102(H102), C22(H22), C218(H218), C111(H111),
 C108(H108), C202(H202), C116(H116), C221(H221), C24(H24), C7(H7), C120(H120),
 C204(H204), C211(H211), C103(H103), C23(H23), C112(H112), C206(H206),
 C216(H216), C110(H110), C12(H12), C11(H11), C208(H208), C122(H122), C17(H17),
 C114(H114), C25(H25), C215(H215), C222(H222), C217(H217), C210(H210), C18(H18),
  C123(H123), C205(H205), C9(H9), C124(H124), C224(H224), C223(H223), C8(H8),
 C19(H19), C121(H121), C209(H209)
3.c Idealised Me refined with riding coordinates:
 C026(H02A,H02B,H02C)
3.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_shelx_res_checksum              25915
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.479
_oxdiff_exptl_absorpt_empirical_full_min 0.720