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_7224367
_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 H86.27 N20 O16 Cd4)'
_chemical_formula_sum            'C38 H37 Cd N7 O6'
_chemical_formula_weight         800.14
_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                 99.84(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.286(5)
_cell_length_b                   18.962(4)
_cell_length_c                   16.247(3)
_cell_measurement_reflns_used    34992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.911
_cell_measurement_theta_min      0.851
_cell_volume                     7372(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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0690
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34459
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.969
_diffrn_reflns_theta_min         0.851
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
 The unit cell contains 16 DMF molecules which 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         1.865
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       0.0120(11)
_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   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         17609
_refine_ls_number_restraints     245
_refine_ls_restrained_S_all      1.213
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.1108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3160
_refine_ls_wR_factor_ref         0.3367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11669
_reflns_number_total             17609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00108d2.cif
_cod_data_source_block           CpdTMU-26
_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_original_formula_sum        'C38 H37 N7 O6 Cd'
_cod_database_code               7224367
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.926
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 N3-C22
 1.32 with sigma of 0.02
 C23-C24 = C24-C25 = C25-C26 = C26-C27 = C27-C28 = C28-C23
 1.39 with sigma of 0.02
 N4-C35 = N8-C59
 1.32 with sigma of 0.02
 C29-C30 = C33-C34 = C47-C48 = C49-C50 = C50-C51
 1.39 with sigma of 0.02
 N3-C24 \\sim N3-C28
 with sigma of 0.02
 N4-C31 \\sim N4-C33
 with sigma of 0.02
 N8-C55 \\sim N8-C57
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N3 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
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
O1 \\sim O2 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C19 \\sim C22: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Others
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H3)=1-FVAR(1)
 Sof(N1)=Sof(H1A)=Sof(H1B)=Sof(H4)=FVAR(1)
 Sof(N10A)=Sof(H11)=1-FVAR(2)
 Sof(N10)=Sof(H10A)=Sof(H10B)=Sof(H12)=FVAR(2)
5.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), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C48(H48),
  C49(H49), C51(H51), C52(H52), C54(H54), C55(H55), C57(H57), C58(H58),
 C61(H61), C62(H62), C63(H63), C64(H64)
5.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N1A(H1AA,H1AB), N10(H10A,H10B)
;
_olex2_submission_special_instructions 'No special instructions were received'