A molecular noble metal-free system for efficient visible light-driven reduction of CO<sub>2</sub> to CO.
Chen, Lingjing; Qin, Yanfei; Chen, Gui; Li, Mingya; Cai, Lirong; Qiu, Yongfu; Fan, Hongbo; Robert, Marc; Lau, Tai-Chu; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9596–9602; doi:10.1039/c9dt00425d

data_7048959
_publ_section_title
;
 A molecular noble metal-free system for efficient visible light-driven
 reduction of CO<sub>2</sub> to CO.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9596
_journal_page_last               9602
_journal_paper_doi               10.1039/c9dt00425d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C35 H24 Fe N6, 2(Cl O4)'
_chemical_formula_sum            'C35 H24 Cl2 Fe N6 O8'
_chemical_formula_weight         783.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2018-09-16 deposited with the CCDC.
2019-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                94.038(3)
_cell_angle_beta                 105.644(4)
_cell_angle_gamma                103.365(4)
_cell_formula_units_Z            2
_cell_length_a                   11.4470(5)
_cell_length_b                   11.5457(5)
_cell_length_c                   13.5944(6)
_cell_measurement_reflns_used    5193
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.6950
_cell_measurement_theta_min      7.9910
_cell_volume                     1666.29(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1270
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega   85.00  177.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000  -60.0000 92

  2 omega  137.00  173.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000 -150.0000 36

  3 omega   90.00  118.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000 -150.0000 28

  4 omega   46.00   72.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -30.0000 26

  5 omega   42.00   69.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000    0.0000 27

  6 omega   43.00   81.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -30.0000 38

  7 omega   40.00  115.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -16.2110 75

  8 omega   88.00  146.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -120.0000 58

  9 omega   80.00  146.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -180.0000 66

 10 omega   77.00  102.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -152.4240 25

 11 omega   44.00   71.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -57.0000 -180.0000 27

 12 omega   43.00   70.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -180.0000 27

 13 omega   40.00   83.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -150.0000 43

 14 omega   37.00   64.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 27

 15 omega   40.00   68.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -120.0000 28

 16 omega   38.00   74.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -120.0000 36

 17 omega    2.00   91.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000 -125.0000 -180.0000 89

 18 omega   34.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -180.0000 28

 19 omega  -11.00   30.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 41

 20 omega  -10.00   80.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -99.0000  -30.0000 90

 21 omega   35.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -30.0000 42

 22 omega   50.00   77.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  150.0000 27

 23 omega   41.00   68.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   30.0000 27

 24 omega   44.00   70.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   60.0000 26

 25 omega   49.00   76.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   90.0000 27

 26 omega   47.00   72.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 25

 27 omega   39.00   72.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 33

 28 omega   41.00  146.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   90.0000 105

 29 omega   85.00  178.00   1.0000   64.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000   30.0000 93

 30 omega   25.00  125.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000   77.0000   60.0000 100

 31 omega  -16.00   98.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -19.0000  -90.0000 114

 32 omega  -69.00  -40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 29

 33 omega  -66.00   12.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000   57.0000 -120.0000 78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0898480000
_diffrn_orient_matrix_UB_12      -0.0519893000
_diffrn_orient_matrix_UB_13      0.0617297000
_diffrn_orient_matrix_UB_21      -0.0800802000
_diffrn_orient_matrix_UB_22      -0.0943647000
_diffrn_orient_matrix_UB_23      -0.0941011000
_diffrn_orient_matrix_UB_31      0.0804252000
_diffrn_orient_matrix_UB_32      -0.0871020000
_diffrn_orient_matrix_UB_33      0.0383071000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12136
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.804
_diffrn_reflns_theta_min         3.410
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.629
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0899P)^2^+2.6781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5798
_reflns_number_total             6344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00425d2.cif
_cod_data_source_block           050817a_jing
_cod_depositor_comments
'Adding full bibliography for 7048959--7048960.cif.'
_cod_original_cell_volume        1666.29(13)
_cod_database_code               7048959
_cell_oxdiff_angle_alpha         94.038(3)
_cell_oxdiff_angle_beta          105.644(4)
_cell_oxdiff_angle_gamma         103.365(4)
_cell_oxdiff_length_a            11.4470(5)
_cell_oxdiff_length_b            11.5457(5)
_cell_oxdiff_length_c            13.5944(6)
_cell_oxdiff_measurement_reflns_used 5193
_cell_oxdiff_volume              1666.29(12)
_reflns_odcompleteness_completeness 96.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.67
_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), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
  C28(H28), C31(H31), C32(H32), C33(H33)
2.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'