A metal-metalloporphyrin framework based on an octatopic porphyrin ligand for chemical fixation of CO<sub>2</sub> with aziridines.
Wang, Xun; Gao, Wen-Yang; Niu, Zheng; Wojtas, Lukasz; Perman, Jason A.; Chen, Yu-Sheng; Li, Zhong; Aguila, Briana; Ma, Shengqian; Chemical communications (Cambridge, England) 54 (2018) 1170–1173; doi:10.1039/c7cc08844b

data_7120967
_publ_section_title
;
 A metal-metalloporphyrin framework based on an octatopic porphyrin ligand
 for chemical fixation of CO<sub>2</sub> with aziridines.
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1170
_journal_page_last               1173
_journal_paper_doi               10.1039/c7cc08844b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '0.25(C400 H208 Cu20 N16 O80)'
_chemical_formula_sum            'C100 H52 Cu5 N4 O20'
_chemical_formula_weight         1947.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_symmetry_space_group_name_Hall  '-I 2 2'
_symmetry_space_group_name_H-M   'I m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2017-10-18 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.294(4)
_cell_length_b                   34.046(6)
_cell_length_c                   34.098(6)
_cell_measurement_reflns_used    7900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      12.7
_cell_measurement_theta_min      2.2
_cell_volume                     30525(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.297
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49594
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.297
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43373
_diffrn_reflns_point_group_measured_fraction_full 0.297
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        17.311
_diffrn_reflns_theta_max         11.442
_diffrn_reflns_theta_min         1.231
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.5955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.424
_exptl_crystal_description       block
_exptl_crystal_F_000             3940
_exptl_crystal_size_max          0.021
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4352
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1518P)^2^+1.0000sin\q] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2606
_reflns_number_total             4352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08844b2.cif
_cod_data_source_block           cu_expboc
_cod_depositor_comments          'Adding full bibliography for 7120967.cif.'
_cod_database_code               7120967
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.997
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C16-C31 = C20-C15
 1.5 with sigma of 0.01
 C24-C31 = C24-C23 = C17-C23 = C17-C12 = C22-C12 = C22-C31 = C15-C4 = C21-C4 =
 C21-C6 = C6-C11 = C14-C11 = C15-C14
 1.39 with sigma of 0.01
 C29-C17 = C6-C9
 1.5 with sigma of 0.01
 C9-C10 = C5-C9 = C8-C5 = C29-C18 = C29-C27 = C30-C27
 1.39 with sigma of 0.01
 C13-C13_$1 = C19-C19_$2 = C32-C32_$3 = C2-C2_$4
 1.35 with sigma of 0.01
 C19-C7 = C13-C1 = C28-C2 = C25-C32
 1.44 with sigma of 0.01
 N4-C28 = N3-C25 = N2-C7 = N1-C1
 1.38 with sigma of 0.01
 C26-C30 = C8-C3
 1.5 with sigma of 0.01
 C26-C28 = C26-C25 = C3-C1 = C3-C7
 1.4 with sigma of 0.01
3. Rigid bond restraints
 C3, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C22, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C30, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C32(H32)
;
_shelx_res_checksum              5507
_olex2_submission_special_instructions 'No special instructions were received'