Nitrogen–nitrogen-functionalized N-heterocyclic carbene ruthenium(ii) complexes realized efficient CO2 hydrogenation to formate
Gong, Huihua; Cui, Tianhua; Liu, Zheyuan; Zheng, Yanling; Zheng, Xueli; Fu, Haiyan; Yuan, Maolin; Chen, Hua; Xu, Jiaqi; Li, Ruixiang; Catalysis Science & Technology 12 (2022) 6213–6218; doi:10.1039/D2CY00741J

data_1567562
_publ_section_title
;
 Nitrogen--nitrogen-functionalized N-heterocyclic carbene ruthenium(ii)
 complexes realized efficient CO2 hydrogenation to formate
;
_journal_issue                   20
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              6213
_journal_page_last               6218
_journal_paper_doi               10.1039/D2CY00741J
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C49 H46 N4 O P2 Ru, 2(B F4)'
_chemical_formula_sum            'C49 H46 B2 F8 N4 O P2 Ru'
_chemical_formula_weight         1043.53
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-01 deposited with the CCDC.	2022-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.285(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0485(5)
_cell_length_b                   17.8373(9)
_cell_length_c                   26.9426(15)
_cell_measurement_reflns_used    4688
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2220
_cell_measurement_theta_min      3.2760
_cell_volume                     4778.7(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -16.00   18.80   0.6000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106  -99.0000    0.0000 58

  2 omega  -81.00    2.40   0.6000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106  -57.0000 -180.0000 139

  3 omega  -82.00  -54.40   0.6000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106  -19.0000 -120.0000 46

  4 omega  -79.00    4.40   0.6000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.8106  -38.0000   90.0000 139
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0373554000
_diffrn_orient_matrix_UB_12      -0.0013688000
_diffrn_orient_matrix_UB_13      -0.0244205000
_diffrn_orient_matrix_UB_21      -0.0607141000
_diffrn_orient_matrix_UB_22      0.0020756000
_diffrn_orient_matrix_UB_23      0.0105108000
_diffrn_orient_matrix_UB_31      0.0019609000
_diffrn_orient_matrix_UB_32      0.0396624000
_diffrn_orient_matrix_UB_33      -0.0014003000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.1091
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            22622
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.056
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         9765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0695P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5993
_reflns_number_total             9765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy00741j2.cif
_cod_data_source_block           190429_s4_ghh
_cod_depositor_comments
'Adding full bibliography for 1567562--1567564.cif.'
_cod_database_code               1567562
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3p3cl1ru1
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.853
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              88523
_olex2_submission_special_instructions 'No special instructions were received'