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_7711696
_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_formula_moiety         'C84 H63 N4 O62 Zn12, 2(C9 H27 Co N3 O6)'
_chemical_formula_sum            'C102 H117 Co2 N10 O74 Zn12'
_chemical_formula_weight         3569.35
_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             2021-04-26
_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                   29.4994(10)
_cell_length_b                   28.8734(9)
_cell_length_c                   17.7149(6)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.19
_cell_volume                     15088.6(9)
_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      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69616
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         2.188
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.179
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1059 before and 0.0696 after correction.
The Ratio of minimum to maximum transmission is 0.7676.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       block
_exptl_crystal_F_000             7220
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.093(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         17235
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+19.3258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                14348
_reflns_number_total             17235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02303b2.cif
_cod_data_source_block           a
_cod_database_code               7711696
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.780
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.907(16)
 0.093(16)
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
3. Restrained distances
 O32-C37
 1.28 with sigma of 0.002
 N2-C48 \\sim N2-C47
 with sigma of 0.02
 Zn7-H30A \\sim Zn7-H30B
 with sigma of 0.02
 O11A-C10 \\sim O11-C10
 with sigma of 0.02
 O6A-C9 \\sim O6-C9
 with sigma of 0.02
 Co1-H35A \\sim Co1-H35B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
O32 \\sim N5 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
O32A \\sim N5A \\sim C37A \\sim C38A \\sim C39A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
O38 \\sim N2 \\sim C46 \\sim C47 \\sim C48: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
O7: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
O34 \\sim N3 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
Uanis(O32A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O11A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O6A) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O11A) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(O32A)=Sof(N5A)=Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=
 Sof(H38F)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(1)
 Sof(O32)=Sof(N5)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(1)
 Sof(O6A)=Sof(O11)=1-FVAR(2)
 Sof(O6)=Sof(O11A)=FVAR(2)
 Sof(Zn1A)=1-FVAR(3)
 Sof(Zn1)=FVAR(3)
 Fixed Sof: H50A(0.5) H50B(0.5) H50C(0.5) C51(0.5) H51A(0.5) H51B(0.5)
 H51C(0.5) H53A(0.5) H53B(0.5) H53C(0.5) H54A(0.5) H54B(0.5) H54C(0.5)
6.a Riding coordinates:
 O00G(H00G), O8(H8), O30(H30A,H30B), C53(H53A,H53B,H53C)
6.b Free rotating group:
 O35(H35A,H35B)
6.c Rotating group:
 O31(H31A,H31B), O36(H36A,H36B), O37(H37B,H37C)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C15(H15), C17(H17), C21(H21), C23(H23),
 C25(H25), C30(H30), C32(H32), C34(H34), C37(H37), C37A(H37A), C49(H49),
 C52(H52), C40(H40), C43(H43), C46(H46)
6.e Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F), C39(H39A,H39B,H39C), C39A(H39D,
 H39E,H39F), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C54(H54A,H54B,H54C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90081
_shelx_fab_checksum              1280
_olex2_submission_special_instructions 'No special instructions were received'