A novel porphyrin MOF catalyst for efficient conversion of CO<sub>2</sub> with propargyl amines.
Zhang, Zhitao; Shen, Kesheng; Zhang, Qian; Duan, Chunying; Jing, Xu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10060–10064; doi:10.1039/d4dt01063a

data_7716303
_publ_section_title
;
 A novel porphyrin MOF catalyst for efficient conversion of CO<sub>2</sub>
 with propargyl amines.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10060
_journal_page_last               10064
_journal_paper_doi               10.1039/d4dt01063a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C48 H25 Cu Fe N4 O9'
_chemical_formula_sum            'C48 H25 Cu Fe N4 O9'
_chemical_formula_weight         921.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-28 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.734(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1724(10)
_cell_length_b                   26.209(2)
_cell_length_c                   23.090(2)
_cell_measurement_reflns_used    4777
_cell_measurement_temperature    250.0
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.35
_cell_volume                     4943.4(8)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      250.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1774
_diffrn_reflns_av_unetI/netI     0.1865
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16161
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.407
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         2.352
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5832
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1623 before and 0.0601 after correction.
The Ratio of minimum to maximum transmission is 0.7822.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_refine_diff_density_max         4.394
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.233
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         7560
_refine_ls_number_restraints     1704
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.1972
_refine_ls_R_factor_gt           0.1352
_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^)+(0.2800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3214
_refine_ls_wR_factor_ref         0.3778
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4616
_reflns_number_total             7560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01063a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7716303.cif.'
_cod_database_code               7716303
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(7)
 0.50(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C02X-C007 = C00J-C007 = C01E-C00B = C01E-C011
 1.45 with sigma of 0.01
 O019-C15
 1.35 with sigma of 0.01
 C7-C1
 1.4 with sigma of 0.01
 C3-C02S
 1.45 with sigma of 0.02
 C16-C02O
 1.45 with sigma of 0.02
 C6-C01E
 1.45 with sigma of 0.02
 C3-C02S = C6-C01E
 1.43 with sigma of 0.02
 C01J-C00V = C01R-C007
 1.4 with sigma of 0.02
 O03B-C16
 1.25 with sigma of 0.02
 C2-C15
 1.45 with sigma of 0.01
 C02P-C00V
 1.45 with sigma of 0.02
 O01B-C00U
 1.35 with sigma of 0.02
 O00F-C00U
 1.25 with sigma of 0.02
 O04K-C16
 1.35 with sigma of 0.02
4. Restrained planarity
 C01E, C011, C00B, Fe01, N00A, N7, N005, N00T
 with sigma of 0.1
 C01E, Fe01, N00T, N005, N7, N00A
 with sigma of 0.1
 C15, C2, C1, Fe01, N00A, N00T, N005, N7, C00M, C00O, C011, C02P, C00J, C00B,
 C02X, C038, C01Y, C00V, C014, C00L, C01E, C01X, C007, C01M, C010, C012, C013,
 C01J, C01R, C024, C020, C02D, C035, C02T, C02E, C045, C03K, C02O, C16, O019,
 O01I, O04K
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
O00F \\sim O019 \\sim O01B \\sim O01I \\sim O04K \\sim O1 \\sim O2 \\sim O03B:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C00M \\sim C01Y \\sim C014 \\sim C00O \\sim C024 \\sim C02T \\sim C2 \\sim C02E
\\sim C020 \\sim C1 \\sim C007 \\sim C00L \\sim C011 \\sim C02P \\sim C01X
\\sim C00U \\sim C00V \\sim C15 \\sim C16 \\sim C01E \\sim C01K \\sim C02N
\\sim C02K \\sim C01J \\sim C016 \\sim C00Q \\sim C01M \\sim C00J \\sim C00B
\\sim C010 \\sim C02D \\sim C045 \\sim C02O \\sim C03K \\sim C035 \\sim C01R
\\sim C02X \\sim C012 \\sim C013 \\sim C038 \\sim C3 \\sim C6 \\sim C03S \\sim
C02M \\sim C02S \\sim C4 \\sim C5 \\sim C7: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O019) \\sim Ueq, Uanis(O01I) \\sim Ueq: with sigma of 0.0001 and sigma
for terminal atoms of 0.0002
Uanis(N00T) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N00T) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.00001 and sigma for
terminal atoms of 0.00002
Uanis(O03B) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(O01B) \\sim Ueq, Uanis(O00F) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma
of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(O04K) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(O04K) \\sim Ueq, Uanis(O03B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C00M) \\sim Ueq, Uanis(C045) \\sim Ueq, Uanis(C016) \\sim Ueq,
Uanis(C01Y) \\sim Ueq, Uanis(C038) \\sim Ueq, Uanis(C014) \\sim Ueq,
Uanis(C00B) \\sim Ueq, Uanis(C00O) \\sim Ueq, Uanis(C01R) \\sim Ueq,
Uanis(C024) \\sim Ueq, Uanis(C02M) \\sim Ueq, Uanis(C02T) \\sim Ueq,
Uanis(C01M) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C02E) \\sim Ueq, Uanis(C03K)
\\sim Ueq, Uanis(C020) \\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C007) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C00L)
\\sim Ueq, Uanis(C00Q) \\sim Ueq, Uanis(C011) \\sim Ueq, Uanis(C00J) \\sim Ueq,
Uanis(C02P) \\sim Ueq, Uanis(C010) \\sim Ueq, Uanis(C01X) \\sim Ueq,
Uanis(C02D) \\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C02O) \\sim Ueq,
Uanis(C00V) \\sim Ueq, Uanis(C035) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C02X)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C013) \\sim Ueq, Uanis(C01E) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C01K) \\sim Ueq, Uanis(C03S) \\sim Ueq, Uanis(C02N)
\\sim Ueq, Uanis(C02S) \\sim Ueq, Uanis(C02K) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C01J) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(N7) \\sim Ueq, Uanis(N00A) \\sim Ueq, Uanis(N00T) \\sim Ueq, Uanis(N005)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Fe01) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of
0.00002
Uanis(O0AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6. Others
 Fixed X: Fe01(0.60964)
 Fixed Y: Fe01(0.556109)
 Fixed Z: Fe01(0.99937)
7.a Aromatic/amide H refined with riding coordinates:
 C01Y(H01Y), C014(H014), C024(H024), C02T(H02T), C02E(H02E), C020(H020),
 C00L(H00L), C01X(H01X), C02N(H02N), C02K(H02K), C016(H016), C00Q(H00Q),
 C01M(H01M), C010(H010), C02D(H02D), C045(H045), C03K(H03K), C035(H035),
 C012(H012), C013(H013), C03S(H03S), C02M(H02M), C4(H4), C5(H5)
7.b Fitted pentagon refined as free rotating group:
 N00A(C00M,C01Y,C014,C00O), C00L(C011,N00T,C02P,C01X), C01M(C00J,N005,C00B,
 C010), C02X(C012,C013,C038,N7)
7.c Fitted hexagon refined as free rotating group:
 C024(C02T,C2,C02E,C020,C1), C01K(C02N,C02K,C01J,C016,C00Q), C02D(C045,C02O,
 C03K,C035,C01R), C6(C03S,C02M,C02S,C4,C5)
7.d Tetrahedral OH refined with riding coordinates:
 O04K(H04K)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98006
_shelx_fab_checksum              39234
_olex2_submission_special_instructions 'No special instructions were received'