Axial Cl/Br atom-mediated CO<sub>2</sub> electroreduction performance in a stable porphyrin-based metal-organic framework.
Huang, Qing; Niu, Qian; Ma, Na-Na; Dong, Long-Zhang; Li, Shun-Li; Li, Dong-Sheng; Cai, Yue-Peng; Lan, Ya-Qian; Chemical communications (Cambridge, England) 56 (2020) 14817–14820; doi:10.1039/d0cc06092e

data_7127481
_publ_section_title
;
 Axial Cl/Br atom-mediated CO<sub>2</sub> electroreduction performance in
 a stable porphyrin-based metal-organic framework.
;
_journal_issue                   94
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14817
_journal_page_last               14820
_journal_paper_doi               10.1039/d0cc06092e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C112 H74.799 Br1.201 Cd3 N24 O0.799'
_chemical_formula_sum            'C112 H74.8 Br1.2 Cd3 N24 O0.8'
_chemical_formula_weight         2202.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-25
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-27 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   47.7736(13)
_cell_length_b                   18.5513(5)
_cell_length_c                   27.2877(8)
_cell_measurement_reflns_used    9648
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.201
_cell_measurement_theta_min      2.76
_cell_volume                     24184.1(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  MX-300
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77485
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            71527
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        27.704
_diffrn_reflns_theta_max         27.825
_diffrn_reflns_theta_min         1.520
_diffrn_source                   synchrotron
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1636 before and 0.1112 after correction.
The Ratio of minimum to maximum transmission is 0.4158.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             8858
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.083
_refine_diff_density_max         2.178
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         11143
_refine_ls_number_restraints     810
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1150P)^2^+92.3866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9943
_reflns_number_total             11143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06092e2.cif
_cod_data_source_block           hq_br1_0ma_sq
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_formula_sum        'C112 H74.80 Br1.20 Cd3 N24 O0.80'
_cod_database_code               7127481
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
C29 \\sim C39 \\sim C28 \\sim C25 \\sim C30 \\sim C56 \\sim C11 \\sim C33 \\sim
C32 \\sim C40 \\sim C15 \\sim C42 \\sim C53 \\sim C31 \\sim C10 \\sim C8 \\sim
C14 \\sim C41 \\sim C43 \\sim C38 \\sim C9 \\sim C4 \\sim C16 \\sim C55 \\sim
C35 \\sim C7 \\sim C34 \\sim C1 \\sim C27 \\sim C54 \\sim C13 \\sim C36 \\sim
C19 \\sim C44 \\sim C26 \\sim C6 \\sim C47 \\sim C12 \\sim C5 \\sim C37 \\sim
C22 \\sim C24 \\sim C23 \\sim C4A \\sim C3A \\sim C51 \\sim C49 \\sim C17A
\\sim C21 \\sim C20 \\sim C48 \\sim C45 \\sim C52A \\sim C18 \\sim C20A \\sim
C21A \\sim C18A \\sim C17 \\sim C50 \\sim C46 \\sim C48A \\sim C49A \\sim C2
\\sim C3 \\sim C45A \\sim C46A \\sim C52 \\sim C50A \\sim C51A \\sim N6 \\sim
N3 \\sim N9 \\sim N12 \\sim N8 \\sim N1 \\sim N2 \\sim N4 \\sim N7 \\sim N5
\\sim N11 \\sim N10A \\sim N10: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
3. Others
 Sof(O1)=Sof(H1A)=0.5*(1-FVAR(2))
 Sof(Br2)=0.5*FVAR(2)
 Fixed Sof: C4A(0.5) H4A(0.5) C3A(0.5) H3A(0.5) N10A(0.5) H10A(0.5) C51(0.5)
 H51(0.5) C49(0.5) H49(0.5) C17A(0.5) H17A(0.5) C21(0.5) H21(0.5) C20(0.5)
 H20(0.5) C48(0.5) H48(0.5) C45(0.5) H45(0.5) C52A(0.5) H52A(0.5) C18(0.5)
 H18(0.5) C20A(0.5) H20A(0.5) C21A(0.5) H21A(0.5) C18A(0.5) H18A(0.5) C17(0.5)
 H17(0.5) C50(0.5) H50(0.5) C46(0.5) H46(0.5) C48A(0.5) H48A(0.5) C49A(0.5)
 H49A(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) C45A(0.5) H45A(0.5) C46A(0.5)
 H46A(0.5) C52(0.5) H52(0.5) C50A(0.5) H50A(0.5) C51A(0.5) H51A(0.5) N10(0.5)
 H10(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C40(H40), C31(H31), C8(H8), C41(H41), C38(H38), C9(H9), C55(H55),
 C35(H35), C34(H34), C1(H1), C27(H27), C54(H54), C13(H13), C36(H36), C26(H26),
 C6(H6), C12(H12), C5(H5), C37(H37), C22(H22), C24(H24), C23(H23), C4A(H4A),
 C3A(H3A), N10A(H10A), C51(H51), C49(H49), C17A(H17A), C21(H21), C20(H20),
 C48(H48), C45(H45), C52A(H52A), C18(H18), C20A(H20A), C21A(H21A), C18A(H18A),
 C17(H17), C50(H50), C46(H46), C48A(H48A), C49A(H49A), C2(H2), C3(H3),
 C45A(H45A), C46A(H46A), C52(H52), C50A(H50A), C51A(H51A), N10(H10)
4.b Tetrahedral OH refined with riding coordinates:
 O1(H1A)
;
_shelx_res_checksum              11507
_shelx_fab_checksum              80165
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'