Two pillared metal‒organic frameworks comprising a long pillar ligand used as fluorescent sensors for nitrobenzene and heterogeneous catalysts for the Knoevenagel condensation reaction
Ghasempour, Hosein; Azhdari Tehrani, Alireza; Morsali, Ali; Wang, Jun; Junk, Peter C.; CrystEngComm 18 (2016) 2463–; doi:10.1039/C6CE00108D

data_7224366
_publ_section_title
;
 Two pillared metal--organic frameworks comprising a long pillar ligand
 used as fluorescent sensors for nitrobenzene and heterogeneous catalysts
 for the Knoevenagel condensation reaction
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2463
_journal_paper_doi               10.1039/C6CE00108D
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.25(C128 H88 N20 O16 Zn4), 0.5(C3 H7 N O)'
_chemical_formula_sum            'C38 H37 N7 O6 Zn'
_chemical_formula_weight         753.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-02-23 deposited with the CCDC.
2016-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.99(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.282(5)
_cell_length_b                   19.029(4)
_cell_length_c                   16.190(3)
_cell_measurement_reflns_used    62905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.954
_cell_measurement_theta_min      1.369
_cell_volume                     7344(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61034
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.369
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
 The unit cell contains 16 DMF molecules and 12 of them have been 
 treated as a diffuse contribution to the overall scattering without 
 specific atom positions by SQUEEZE/PLATON.

 Ref: Spek, A.L. (1990), Acta Cryst. A46, C-34;
 Spek, A.L. (2009), Acta Cryst. D65, 148-155
;
_refine_diff_density_max         1.669
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0060(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     843
_refine_ls_number_reflns         16518
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.1046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+32.1625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2586
_refine_ls_wR_factor_ref         0.2651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13498
_reflns_number_total             16518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00108d2.cif
_cod_data_source_block           CpdTMU-25
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7224366--7224367.cif.
;
_cod_database_code               7224366
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C53-C54 = C54-C55 = C55-C56 = C56-C57 = C57-C58 = C58-C53
 1.39 with sigma of 0.02
 C59-C60 = N8-C47 = N9-C56
 1.5 with sigma of 0.02
 N9-C59
 1.32 with sigma of 0.02
 N9-C55 \\sim N9-C57
 with sigma of 0.02
3. Restrained planarity
 C53, C54, C55, C56, C57, C58
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O9 \\sim N11 \\sim C100 \\sim C101 \\sim C102: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
N8 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim
C53: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
N9 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim
C60: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C59 \\sim C60: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
N5 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N9) \\sim Ueq, Uanis(C201) \\sim Ueq, Uanis(C202) \\sim Ueq: with sigma
of 0.03 and sigma for terminal atoms of 0.06
Uanis(C51) = Uanis(C52)
Uanis(C55) = Uanis(C53)
5. Others
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H3)=1-FVAR(1)
 Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(H4)=FVAR(1)
 Sof(N2A)=Sof(H2AA)=Sof(H2AB)=Sof(H11)=1-FVAR(2)
 Sof(N2)=Sof(H2A)=Sof(H2B)=Sof(H12)=FVAR(2)
 Sof(C200)=Sof(H200)=Sof(C201)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C202)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(3)
 Sof(C100)=Sof(H100)=Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C102)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27),
  C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C48(H48),
  C49(H49), C51(H51), C52(H52), C54(H54), C55(H55), C57(H57), C58(H58),
 C61(H61), C62(H62), C63(H63), C64(H64), C100(H100), C200(H200)
6.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N1A(H1AA,H1AB), N2(H2A,H2B), N2A(H2AA,H2AB)
6.c Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C201(H20A,H20B,H20C), C202(H20D,
 H20E,H20F)
;
_olex2_submission_special_instructions 'No special instructions were received'