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_7129879
_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(Cl O4)'
_chemical_formula_sum            'C27 H25 Cl2 N7 O8 Ru'
_chemical_formula_weight         747.51
_chemical_name_systematic        RuC(ClO4)2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-17 deposited with the CCDC.	2022-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                86.015(2)
_cell_angle_beta                 85.355(2)
_cell_angle_gamma                68.961(2)
_cell_formula_units_Z            4
_cell_length_a                   10.6790(2)
_cell_length_b                   12.5659(3)
_cell_length_c                   23.1366(5)
_cell_measurement_reflns_used    29277
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      31.3140
_cell_measurement_theta_min      1.9240
_cell_volume                     2885.51(11)
_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_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.833
_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     44.00  84.00   0.50    1.80    --   11.21-178.00 -30.00   80
  2  \w     52.00  90.00   0.50    1.80    --   11.21-178.00 -60.00   76
  3  \w     45.00  85.00   0.50    1.80    --   11.21-178.00-150.00   80
  4  \w    -18.00   8.00   0.50    1.80    --  -12.77 -99.00   0.00   52
  5  \w    -18.00  15.00   0.50    1.80    --  -12.77 -99.00 -90.00   66
  6  \w     -9.00  19.00   0.50    1.80    --  -12.77 -99.00-180.00   56
  7  \w    -18.00   7.00   0.50    1.80    --  -12.77 -99.00-120.00   50
  8  \w    -71.00 -43.00   0.50    1.80    --  -12.77-178.00-120.00   56
  9  \w    -69.00 -43.00   0.50    1.80    --  -12.77-178.00  60.00   52
 10  \w    -89.00   6.00   0.50    1.80    --  -12.77 -43.00  20.00  190
 11  \w    -24.00  63.00   0.50    1.80    --  -12.77  43.00 171.00  174
 12  \w    -91.00 -41.00   0.50    1.80    --  -12.77 178.00 -90.00  100
 13  \w    -92.00 -42.00   0.50    1.80    --  -12.77 178.00-150.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0616104000
_diffrn_orient_matrix_UB_12      0.0098110000
_diffrn_orient_matrix_UB_13      -0.0016024000
_diffrn_orient_matrix_UB_21      0.0298879000
_diffrn_orient_matrix_UB_22      -0.0518318000
_diffrn_orient_matrix_UB_23      0.0162217000
_diffrn_orient_matrix_UB_31      0.0198409000
_diffrn_orient_matrix_UB_32      -0.0296939000
_diffrn_orient_matrix_UB_33      -0.0261178000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48274
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.412
_diffrn_reflns_theta_min         1.915
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.634
_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            'dark red'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.076
_refine_diff_density_max         2.164
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         15899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12865
_reflns_number_total             15899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00657j2.cif
_cod_data_source_block           ruc(clo4)
_cod_database_code               7129879
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C27 N7 H25 Ru Cl2 O8'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C01D(H01A,H01B), C01F(H01C,H01D)
2.b Aromatic/amide H refined with riding coordinates:
 C014(H014), C016(H016), C017(H017), C01E(H01E), C01G(H01G), C01I(H01I),
 C01K(H01K), C01L(H01L), C01M(H01M), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y),
 C01Z(H01Z), C020(H020), C021(H021), C023(H023), C024(H024), C025(H025),
 C026(H026), C027(H027), C028(H028), C029(H029), C02B(H02G), C02C(H02H),
 C02D(H02I), C02E(H02J), C02F(H02K), C02G(H02L)
2.c Idealised Me refined as rotating group:
 C022(H02A,H02B,H02C), C02A(H02D,H02E,H02F), C02H(H02M,H02N,H02O), C02I(H02P,
 H02Q,H02R)
;
_shelx_res_checksum              4414
_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 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.692