Gas–solid two-phase flow method for preparing trimesic acid series MOFs for catalytic thermal decomposition of ammonium perchlorate
Zhang, Juan; Zhao, Jun; Jin, Bo; Peng, Rufang; Dalton Transactions  (2022) –; doi:10.1039/D2DT02303B

data_7711695
_publ_section_title
;
 Gas--solid two-phase flow method for preparing trimesic acid series MOFs
 for catalytic thermal decomposition of ammonium perchlorate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02303B
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C84 H62 N4 O59 Zn12, C9 H27 N3 O6 Zn, 0.5(H6 O2)'
_chemical_formula_sum            'C93 H92 N7 O66 Zn13'
_chemical_formula_weight         3213.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-10 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.577(8)
_cell_length_b                   28.974(8)
_cell_length_c                   17.758(5)
_cell_measurement_reflns_used    9654
_cell_measurement_temperature    193
_cell_measurement_theta_max      26.936
_cell_measurement_theta_min      2.278
_cell_volume                     15218(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53549
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.599
_diffrn_reflns_theta_min         1.511
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.092
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0901 after correction.
The Ratio of minimum to maximum transmission is 0.7220.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             6468
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.058(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         17753
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1475P)^2^+44.6568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                14814
_reflns_number_total             17753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02303b2.cif
_cod_data_source_block           b_sq
_cod_database_code               7711695
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.787
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.942(18)
 0.058(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
3. Restrained distances
 C11-N1
 1.4 with sigma of 0.02
 N2-C54
 1.46 with sigma of 0.02
 N2-C53
 1.45 with sigma of 0.02
 C52-N2
 1.36 with sigma of 0.02
 C52-O13
 1.22 with sigma of 0.02
 C52-C53
 2.46 with sigma of 0.04
 C52-C54
 2.45 with sigma of 0.04
 N3-C23 \\sim N3-C22
 with sigma of 0.02
 O22A-C39 \\sim O22-C39
 with sigma of 0.02
 N5-C27 \\sim N5-C26
 with sigma of 0.02
 N2-C53 \\sim N2-C54
 with sigma of 0.02
 Zn8-H34B \\sim Zn8-H34A
 with sigma of 0.02
 N4-C30 \\sim N4-C29
 with sigma of 0.02
4. Restrained planarity
 C52, O13, N2, C53, C54
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
O1 \\sim C10 \\sim N1 \\sim C12 \\sim C11: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
O22A \\sim O22: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
O31 \\sim C49 \\sim N01J \\sim C50 \\sim C51: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C52 \\sim O13 \\sim N2 \\sim C53 \\sim C54: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O35 \\sim C28 \\sim C29 \\sim N4 \\sim C30: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
O37 \\sim C24 \\sim N3 \\sim C22 \\sim C23: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C52 \\sim C54 \\sim N2 \\sim C53 \\sim O13: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C25 \\sim N5 \\sim C27 \\sim C26 \\sim O33: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
O27 \\sim C48 \\sim O26: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O27) \\sim Ueq, Uanis(O32) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O22) \\sim Ueq, Uanis(O22A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
6. Rigid body (RIGU) restrains
 C52, O13, N2, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(Zn6A)=1-FVAR(1)
 Sof(H30A)=0.5*(1-FVAR(2))
 Sof(H30)=0.5*FVAR(2)
 Sof(Zn6)=FVAR(1)
 Sof(O22A)=1-FVAR(2)
 Sof(O22)=FVAR(2)
 Sof(Zn2A)=Sof(H3B)=1-FVAR(3)
 Sof(Zn2)=Sof(H3A)=FVAR(3)
 Fixed Sof: Zn8(0.5) O38(0.5) H38A(0.5) H38B(0.5) O36(0.5) H36A(0.5) H36B(0.5)
 O37(0.5) O34(0.5) H34A(0.5) H34B(0.5) O33(0.5) N5(0.5) N3(0.5) O35(0.5)
 C25(0.5) H25(0.5) N4(0.5) C24(0.5) H24(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
 H51A(0.5) H51B(0.5) H51C(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C26(0.5)
 H26A(0.5) H26B(0.5) H26C(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C23(0.5)
 H23A(0.5) H23B(0.5) H23C(0.5) C28(0.5) H28(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) C30(0.5) H30B(0.5) H30C(0.5) H30D(0.5) H32B(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) H53C(0.5) H54A(0.5) H54B(0.5) H54C(0.5) H39A(0.5) H39B(0.5) H39C(0.5)
8.a Riding coordinates:
 O38(H38A,H38B), O2(H2A,H2B), O36(H36A,H36B), O34(H34A,H34B), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C12(H12A,H12B,H12C), C30(H30B,H30C,H30D), O32(H32A,
 H32B), C53(H53A,H53B,H53C), O39(H39A,H39B,H39C)
8.b Ternary CH refined with riding coordinates:
 O10(H10), O30(H30), O30(H30A), O3(H3A), O3(H3B)
8.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C33(H33), C3(H3), C19(H19), C15(H15), C46(H46), C17(H17), C44(H44),
 C5(H5), C7(H7), C42(H42), C35(H35), C49(H49), C25(H25), C24(H24), C10(H10A),
 C28(H28), C52(H52)
8.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C29(H29A,H29B,H29C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              52118
_shelx_fab_checksum              72642
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'