Urea-containing metal-organic frameworks as heterogeneous organocatalysts
Tehrani, Alireza Azhdari; Abedi, Sedigheh; Morsali, Ali; Wang, Jun; Junk, Peter C.; Journal of Materials Chemistry A 3 (2015) 20408–; doi:10.1039/C5TA03835A

data_7236080
_publ_section_title
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 Urea-containing metal-organic frameworks as heterogeneous organocatalysts
;
_journal_issue                   40
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              20408
_journal_paper_doi               10.1039/C5TA03835A
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety         'C21 H16 N3 O5 Zn'
_chemical_formula_sum            'C21 H16 N3 O5 Zn'
_chemical_formula_weight         455.74
_chemical_name_systematic        TMU-19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-01-04 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.035(4)
_cell_length_b                   16.064(3)
_cell_length_c                   29.891(6)
_cell_measurement_temperature    100(2)
_cell_volume                     10100(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            81323
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.439
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.975
_exptl_transmission_factor_min   0.942
_platon_squeeze_details
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.029(2)
_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   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         11539
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1695P)^2^+1.4959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2428
_refine_ls_wR_factor_ref         0.2532
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8725
_reflns_number_total             11539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ta03835a2.cif
_cod_data_source_block           TMU-19
_cod_database_code               7236080
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.942
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C17-C21 \\sim C16-C22
 with sigma of 0.02
 C19-C21 \\sim C20-C22
 with sigma of 0.02
 C17-C23 \\sim C16-C24
 with sigma of 0.02
3. Restrained planarity
 N3, C21, C22, C23, C24, C18, C25
 with sigma of 0.1
4. Others
 Fixed Sof: C19(0.5) H19(0.5) C20(0.5) H20(0.5) C24(0.5) H24(0.5) C16(0.5)
 H16(0.5) C17(0.5) H17(0.5) C23(0.5) H23(0.5) C22(0.5) H22(0.5) C21(0.5)
 H21(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C3(H3), C10(H10), N1(H1), C13(H13), N2(H2), C7(H7), C6(H6), C4(H4),
 C19(H19), C20(H20), C14(H14), C24(H24), C16(H16), C17(H17), C23(H23), C22(H22),
  C21(H21)
;
_olex2_submission_special_instructions 'No special instructions were received'