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_7125383
_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         'C28 H32 Cl2 Fe2 N8 O, 2(Cl)'
_chemical_formula_sum            'C28 H32 Cl4 Fe2 N8 O'
_chemical_formula_weight         750.11
_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             2018-11-17
_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                98.812(2)
_cell_angle_beta                 92.127(2)
_cell_angle_gamma                91.893(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1131(16)
_cell_length_b                   11.477(2)
_cell_length_c                   18.784(3)
_cell_measurement_reflns_used    8331
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.111
_cell_measurement_theta_min      2.238
_cell_volume                     1938.6(6)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22027
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.170
_diffrn_reflns_theta_min         1.098
_diffrn_source                   'rotating-anode with a mirror focussing unit'
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.0805 before and 0.0503 after correction. The Ratio 
of minimum to maximum transmission is 0.7501. The \l/2 correction 
factor is 0.00150.'
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_recrystallization_method
'slow diffusion of diethylether into a solution of the compound in methanol'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         8518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0765P)^2^+3.2975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6793
_reflns_number_total             8518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04191e2.cif
_cod_data_source_block           yuto_feh_3_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               7125383
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.833
_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), C20(H20A,H20B),
 C21(H21A,H21B), C27(H27A,H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4A), C9(H9), C10(H10), C11(H11), C16(H16), C17(H17),
 C18(H18), C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              28385
_shelx_fab_checksum              62259
_olex2_submission_special_instructions 'No special instructions were received'