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_7711694
_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         'C45 H51 Co3 N6 O24'
_chemical_formula_sum            'C45 H51 Co3 N6 O24'
_chemical_formula_weight         1236.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-24
_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                 90.0070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6590(6)
_cell_length_b                   14.1439(5)
_cell_length_c                   28.8454(10)
_cell_measurement_reflns_used    5012
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.329
_cell_measurement_theta_min      2.924
_cell_volume                     6796.6(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.1099
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            24857
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.868
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 91227 reflections, Rint = 0.1000
 (31349 with I > 3sig(I), Rint = 0.0720)
;
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.857
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         12434
_refine_ls_number_restraints     900
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.1353
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+107.7526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3346
_refine_ls_wR_factor_ref         0.3494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9187
_reflns_number_total             12434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02303b2.cif
_cod_data_source_block           t_a_sq
_cod_database_code               7711694
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.656(3)
 0.344(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-C2
 1.45 with sigma of 0.001
 C41-N6
 1.45 with sigma of 0.001
 N4-C28 \\sim N4-C29
 with sigma of 0.02
 N2-C6 \\sim N2-C4
 with sigma of 0.02
 N5-C43 \\sim N5-C44
 with sigma of 0.02
 N1-C2 \\sim N1-C3
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C014) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C28)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C36) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O21) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C22(H22), C24(H24), C20(H20), C32(H32), C34(H34), C014(H014),
 C11(H11), C9(H9), C42(H42), C15(H15), C5(H5), C27(H27), C39(H39), C1(H1)
6.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C28(H28A,H28B,H28C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C29(H29A,H29B,H29C), C17(H17A,H17B,H17C), C6(H6A,H6B,
 H6C), C2(H2A,H2B,H2C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              58661
_shelx_fab_checksum              12546
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'