An earth-abundant system for light-driven CO<sub>2</sub> reduction to CO using a pyridinophane iron catalyst.
Sakaguchi, Yuto; Call, Arnau; Cibian, Mihaela; Yamauchi, Kosei; Sakai, Ken; Chemical communications (Cambridge, England) 55 (2019) 8552–8555; doi:10.1039/c9cc04191e

data_7125381
_publ_section_title
;
 An earth-abundant system for light-driven CO<sub>2</sub> reduction to CO
 using a pyridinophane iron catalyst.
;
_journal_issue                   59
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8552
_journal_page_last               8555
_journal_paper_doi               10.1039/c9cc04191e
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C14 H16 Cl2 Co N4, Cl'
_chemical_formula_sum            'C14 H16 Cl3 Co N4'
_chemical_formula_weight         405.59
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-21 deposited with the CCDC.	2019-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                93.6550(10)
_cell_angle_beta                 98.8980(10)
_cell_angle_gamma                90.0060(10)
_cell_formula_units_Z            2
_cell_length_a                   9.1082(10)
_cell_length_b                   9.8312(10)
_cell_length_c                   9.9666(11)
_cell_measurement_reflns_used    7067
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.036
_cell_measurement_theta_min      2.264
_cell_volume                     879.88(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10731
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.088
_diffrn_reflns_theta_min         2.073
_diffrn_source                   'rotating-anode with a mirror focussing unit'
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.0772 before and 0.0376 after correction. The Ratio 
of minimum to maximum transmission is 0.7914. The \l/2 correction 
factor is 0.00150.'
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_recrystallization_method
'slow diffusion of diethylether into a solution of the compound in methanol'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         4301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.5539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3861
_reflns_number_total             4301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04191e2.cif
_cod_data_source_block           yuto_co_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7125381
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11)
;
_shelx_res_checksum              79425
_shelx_fab_checksum              21724
_olex2_submission_special_instructions 'No special instructions were received'