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_7127480
_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 H72.531 Cd3 Cl1.469 N24 O0.531'
_chemical_formula_sum            'C112 H72.53 Cd3 Cl1.47 N24 O0.53'
_chemical_formula_weight         2152.21
_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                   47.491(2)
_cell_length_b                   18.5114(10)
_cell_length_c                   27.2738(13)
_cell_measurement_reflns_used    5717
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.22
_cell_measurement_theta_min      2.481
_cell_volume                     23977(2)
_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)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  MX-300
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77485
_diffrn_reflns_av_R_equivalents  0.1285
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            79777
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        27.704
_diffrn_reflns_theta_max         28.573
_diffrn_reflns_theta_min         0.935
_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    0.770
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 110222 reflections, Rint = 0.1993
 (58883 with I > 3sig(I), Rint = 0.1657)
;
_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    1.192
_exptl_crystal_description       block
_exptl_crystal_F_000             8686
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         11698
_refine_ls_number_restraints     756
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+398.3530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7914
_reflns_number_total             11698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06092e2.cif
_cod_data_source_block           hq_cl3_0ma_sq
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7127480
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.884
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C19
\\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29
\\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37
\\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C47
\\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C17A \\sim C18A \\sim C19A \\sim
C20A \\sim C45A \\sim C46A \\sim C48A \\sim C49A \\sim C50 \\sim C51 \\sim C52
\\sim C17 \\sim C18 \\sim C20 \\sim C21 \\sim C45 \\sim C46 \\sim C48 \\sim C49
\\sim C51A \\sim C50A \\sim C52A \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5
\\sim N6 \\sim N7 \\sim N8 \\sim N9 \\sim N12 \\sim N10 \\sim N10A \\sim N11:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=1-
 FVAR(1)
 Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=
 Sof(H49A)=FVAR(1)
 Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=1-
 FVAR(2)
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(H20A)=FVAR(2)
 Sof(C51A)=Sof(H51A)=Sof(N10A)=Sof(C50A)=Sof(H50A)=Sof(C52A)=Sof(H52A)=1-FVAR(3)
 Sof(N10)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=FVAR(3)
 Sof(O1)=Sof(H1A)=0.5*(1-FVAR(5))
 Sof(Cl2)=0.5*FVAR(5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C31(H31), C32(H32), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C54(H54),
 C55(H55), C17A(H17A), C18A(H18A), C19A(H19A), C20A(H20A), C45A(H45A),
 C46A(H46A), C48A(H48A), C49A(H49A), C50(H50), C51(H51), C52(H52), C17(H17),
 C18(H18), C20(H20), C21(H21), C45(H45), C46(H46), C48(H48), C49(H49),
 C51A(H51A), C50A(H50A), C52A(H52A)
4.b Fitted pentagon refined as free rotating group:
 C51A(N10A,C50A,N11,C52A)
4.c Tetrahedral OH refined with riding coordinates:
 O1(H1A)
;
_shelx_res_checksum              48649
_shelx_fab_checksum              62464
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'