Ugi's amine based coordination polymers as synergistic catalysts for the electrocatalytic reduction of carbon dioxide.
Khrizanforov, Mikhail N.; Naileva, Farida F.; Ivshin, Kamil A.; Zagidullin, Almaz A.; Samorodnova, Anastasiia P.; Milyukova, Polina V.; Shekurov, Ruslan P.; Laskin, Artem I.; Novikov, Alexander S.; Miluykov, Vasily A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17351–17360; doi:10.1039/d4dt01181c

data_7717128
_publ_section_title
;
 Ugi's amine based coordination polymers as synergistic catalysts for the
 electrocatalytic reduction of carbon dioxide.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17351
_journal_page_last               17360
_journal_paper_doi               10.1039/d4dt01181c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H31 Co Fe N5 O4 P2'
_chemical_formula_sum            'C32 H31 Co Fe N5 O4 P2'
_chemical_formula_weight         726.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-28 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.368(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9939(16)
_cell_length_b                   11.4106(9)
_cell_length_c                   21.1115(16)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.64
_cell_volume                     4606.8(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v2018.1-0'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22119
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.823
_diffrn_reflns_theta_min         1.785
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.609282
_exptl_absorpt_correction_T_min  0.211800
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1373 before and 0.0882 after correction.
 
For component 2:
 wR2(int) was 0.1454 before and 0.0980 after correction.
 The Ratio of minimum to maximum transmission is 0.69.

Final HKLF 4 output contains 112234 reflections, Rint = 0.1119
 (52051 with I > 3sig(I), Rint = 0.0807)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_description       prism
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.531
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.202
_refine_diff_density_max         3.155
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.320
_refine_ls_extinction_coef       0.058(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   2.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         22119
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      2.292
_refine_ls_R_factor_all          0.2297
_refine_ls_R_factor_gt           0.1947
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5237
_refine_ls_wR_factor_ref         0.5443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16030
_reflns_number_total             22119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01181c2.cif
_cod_data_source_block           zag001_12345
_cod_depositor_comments          'Adding full bibliography for 7717128.cif.'
_cod_database_code               7717128
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.454(4)
 0.546(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C17-C16
 1.29 with sigma of 0.002
 C15-C17
 2.17 with sigma of 0.005
 C16-C18
 2.17 with sigma of 0.005
 C16-C15
 1.43 with sigma of 0.01
 C18-C17
 1.43 with sigma of 0.01
 C14-C15
 1.43 with sigma of 0.01
 C14-C18
 1.43 with sigma of 0.01
 C16-C17
 1.42 with sigma of 0.002
 C15-C16
 1.42 with sigma of 0.002
 C15-C18
 2.34 with sigma of 0.005
 C20-C21
 2.47 with sigma of 0.005
 N19-C20
 1.51 with sigma of 0.005
 N19-C21
 1.51 with sigma of 0.005
 C10-C9 \\sim C11-C10
 with sigma of 0.005
 C13-C9 \\sim C12-C13
 with sigma of 0.005
4. Restrained planarity
 C14, C15, C16, C17, C18
 with sigma of 0.005
 C9, C10, C11, C12, C13
 with sigma of 0.005
5. Uiso/Uaniso restraints and constraints
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.003 within 2A
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.003 within 2A
N19 \\sim C13: within 2A with sigma of 0.003 and sigma for terminal atoms of
0.002 within 2A
P2: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.003 within
2A
P1 \\sim O1: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.004 within 2A
C2 \\sim C3 \\sim C4: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.004 within 2A
Uanis(Co1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(N5) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.003
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.004
Uanis(N1) = Uanis(N5)
Uanis(C3) = Uanis(C30)
Uanis(C8) = Uanis(C25)
Uanis(N5) = Uanis(N1) = Uanis(N22) = Uanis(N28)
Uanis(C23) = Uanis(C24) = Uanis(C26) = Uanis(C27)
Uanis(C21) = Uanis(C20)
Uanis(C40) = Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C41) = Uanis(C39) =
Uanis(N38)
Uanis(C33) = Uanis(C30) = Uanis(C31) = Uanis(C32) = Uanis(C29)
Uanis(N38) = Uanis(N34)
6. Rigid body (RIGU) restrains
 C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N19, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Ternary CH refined with riding coordinates:
 N19(H19), C12(H12), C14(H14), C17(H17)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C15(H15), C16(H16),
 C18(H18), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32),
  C33(H33), C35(H35), C36(H36), C39(H39), C40(H40)
7.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24049
_shelx_hkl_checksum              65514
_shelx_fab_checksum              33850
_olex2_submission_special_instructions 'No special instructions were received'