A 3D/3D hetero-interpenetrated MOF with a novel (3,9)-c net and 6-c lcy net for the fluorescence detection of carbaryl
Shi, Rong; Xu, Ze-Ming; Chen, Cao; Niu, Zheng; Lang, Jian-Ping; Dalton Transactions  (2022) –; doi:10.1039/D2DT01893D

data_7711367
_publ_section_title
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 A 3D/3D hetero-interpenetrated MOF with a novel (3,9)-c net and 6-c lcy
 net for the fluorescence detection of carbaryl
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01893D
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety
'C327 H214 N27 O110 Zn16, C156 H96 N12 O50 Zn8, 3(Cl O4), 1(C4 H12 N), 6[C5H11NO], 14[H2O]'
_chemical_formula_sum            'C517 H416 Cl3 N46 O192 Zn24'
_chemical_formula_weight         12021.111
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_Int_Tables_number      198
_audit_block_doi                 10.5517/ccdc.csd.cc27vz14
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.07.25 svn.r36e0af09 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2022-09-25 deposited with the CCDC.	2022-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.520(5)
_cell_length_b                   32.520(5)
_cell_length_c                   32.520(5)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    119.97
_cell_measurement_theta_max      24.07
_cell_measurement_theta_min      2.26
_cell_volume                     34392(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      119.97
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.9986
_diffrn_reflns_Laue_measured_fraction_max 0.9986
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            94763
_diffrn_reflns_point_group_measured_fraction_full 0.9987
_diffrn_reflns_point_group_measured_fraction_max 0.9987
_diffrn_reflns_theta_full        24.7426
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             12320.190
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.5488
_refine_diff_density_min         -0.6577
_refine_diff_density_rms         0.0951
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.026(6)
_refine_ls_d_res_high            0.8491
_refine_ls_d_res_low             10.2837
_refine_ls_goodness_of_fit_ref   0.9892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    129
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         19628
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.9882
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          -0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0976P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1514
_reflns_Friedel_coverage         0.999
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              38
_reflns_limit_k_min              -38
_reflns_limit_l_max              38
_reflns_limit_l_min              -38
_reflns_number_gt                16622
_reflns_number_total             19628
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt01893d2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     ' P 2ac 2ab 3'
_cod_database_code               7711367
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C85-C84
 1.5 with sigma of 0.02
 N6-C85
 1.5 with sigma of 0.02
 C56-C57
 1.5 with sigma of 0.02
 C54-C55
 1.5 with sigma of 0.02
 H4Ba-O4B
 0.9 with sigma of 0.02
 H4Bb-O4B
 0.9 with sigma of 0.02
 C53-N5
 1.5 with sigma of 0.02
 C87-C86
 1.5 with sigma of 0.02
 C86-N6
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C55 \\sim C54 \\sim N5 \\sim C53 \\sim C56 \\sim C57 \\sim Zn6: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O4A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(O4B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.01
Uanis(C86) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C87) = Uanis(C86) = Uanis(N6) = Uanis(C85) = Uanis(C84)
Uanis(N5) = Uanis(C54) = Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C53)
Uanis(O4B) = Uanis(O4A)
Uanis(O1) = Uanis(O2)
4. Others
 Fixed Sof: Cl2(0.166667) H1a(0.33333) H1b(0.33333) O32(0.166667) O4B(0.5)
 H4Ba(0.5) H4Bb(0.5) O33(0.5) N5(0.5) C53(0.5) C57(0.5) H57a(0.5) H57b(0.5)
 H57c(0.5) C56(0.5) C54(0.5) C55(0.5) H55a(0.5) H55b(0.5) H55c(0.5) N6(0.16667)
 H6a(0.16667) H6b(0.16667) C84(0.16667) H84a(0.16667) H84b(0.16667)
 H84c(0.16667) C85(0.16667) H85a(0.16667) H85b(0.16667) C86(0.16667)
 H86a(0.16667) H86b(0.16667) C87(0.16667) H87a(0.16667) H87b(0.16667)
 H87c(0.16667) O4A(0.5)
5.a Riding coordinates:
 C57(H57a,H57b,H57c), C84(H84a,H84b,H84c), C55(H55c,H55b,H55a)
5.b Ternary CH refined with riding coordinates:
 O12(H12), C12(H12a), C11(H11), C10(H10), C38(H38), C15(H15), C16(H16),
 C17(H17), C37(H37), C42(H42), C41(H41), C43(H43), C36(H36), C73(H73), C72(H72),
  C69(H69), C67(H67), C74(H74), C71(H71)
5.c Secondary CH2 refined with riding coordinates:
 N6(H6a,H6b), C85(H85a,H85b), C86(H86a,H86b)
5.d Aromatic/amide H refined with riding coordinates:
 C50(H50), C51(H51), C25(H25), C24(H24), C48(H48), C14(H14), C79(H79),
 C13(H13), C77(H77), C80(H80), C21(H21), C47(H47), C39(H39), C22(H22), C33(H33),
  C82(H82), C6(H6), C61(H61), C40(H40), C60(H60), C4(H4), C70(H70), C29(H29),
 C30(H30), C68(H68), C32(H32), C63(H63), C64(H64)
5.e X=CH2 refined with riding coordinates:
 O1(H1a,H1b), O4B(H4Ba,H4Bb)
5.f Idealised Me refined as rotating group:
 C87(H87a,H87b,H87c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 944 electrons were 
found in a volume of 12368\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 6[C5H11NO], 14[H2O] per Formula Unit 
which account for 952 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'