An anthracene-based microporous metal–organic framework for adsorbing CO2 and detecting TNP sensitivity
An, Qingbo; Bao, Siqi; Li, Xiao; Sun, Jing; Su, Zhongmin; New Journal of Chemistry 46 (2022) 11377–11381; doi:10.1039/D2NJ02015G

data_7061506
_publ_section_title
;
 An anthracene-based microporous metal--organic framework for adsorbing
 CO2 and detecting TNP sensitivity
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11377
_journal_page_last               11381
_journal_paper_doi               10.1039/D2NJ02015G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety
'C100 H66 Cd3 N14 O19, C4 H9 N O, 3[C4H9NO], 10[H2O]'
_chemical_formula_sum            'C116 H122 Cd3 N18 O33'
_chemical_formula_weight         2633.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-11
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-15 deposited with the CCDC.	2022-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                73.8090(10)
_cell_angle_beta                 68.6360(10)
_cell_angle_gamma                73.2410(10)
_cell_formula_units_Z            2
_cell_length_a                   16.4608(9)
_cell_length_b                   19.5414(11)
_cell_length_c                   21.2468(12)
_cell_measurement_reflns_used    5921
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_cell_volume                     5977.6(6)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34574
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.564
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         21043
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12567
_reflns_number_total             21043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02015g2.cif
_cod_data_source_block           CUST-607
_cod_depositor_comments          'Adding full bibliography for 7061506.cif.'
_cod_database_code               7061506
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.02
 H1WA-H1WB
 1.34 with sigma of 0.04
 Cd3-H1WA \\sim Cd3-H1WB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cd3 \\sim N4 \\sim O1W \\sim O16: within 3.2A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 3.2A
O19 \\sim C90: within 3.2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 3.2A
Uanis(O18) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C37) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(N16) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(O19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: N6(0.5) H6(0.5) N11(0.5) H11(0.5) C4(0.5) H13B(0.5) H13A(0.5)
 H35A(0.5) H35(0.5) C37(0.5) O18(0.25) N16(0.5) H16A(0.5) C105(0.5) O22(0.75)
 C106(0.5) N17(0.5) H17(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N6(H6), N9(H9), N10(H10), N11(H11), N12(H12), N13(H13), C11(H11A), C13(H13B),
 C13(H13A), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C25(H25), C26(H26), C35(H35A), C35(H35), C38(H38),
 C39(H39), C47(H47), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C56(H56),
  C59(H59), C60(H60), C61(H61), C64(H64), C66(H66), C67(H67), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76),
  C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87), C89(H89), C91(H91), C92(H92), C93(H93), C94(H94),
  C95(H95), C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), N16(H16A),
 N17(H17)
5.b Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C103(H10D,H10E,H10F), C104(H10G,H10H,H10I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 501 electrons were 
found in a volume of 1821\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
3[C4H9NO],10[H2O] per Asymmetric Unit 
which account for 480 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18291
_shelx_fab_checksum              25879
_olex2_submission_special_instructions 'No special instructions were received'