Design and synthesis of squaramide-based MOFs as efficient MOF-supported hydrogen-bonding organocatalysts
Xiaoping Zhang; Zhenjie Zhang; Jake Boissonnault; Seth M. Cohen; Chem.Commun. 52 (2016) 8585–; doi:

data_7119827
_publ_section_title
;
 Design and synthesis of squaramide-based MOFs as efficient MOF-supported
 hydrogen-bonding organocatalysts
;
_journal_name_full               Chem.Commun.
_journal_page_first              8585
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C180 H54 N18 O108 Zn18'
_chemical_formula_sum            'C180 H54 N18 O108 Zn18'
_chemical_formula_weight         5373.77
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-05 deposited with the CCDC.
2016-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   18.816(2)
_cell_length_b                   18.816(2)
_cell_length_c                   38.416(5)
_cell_measurement_reflns_used    2915
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.01
_cell_measurement_theta_min      2.46
_cell_volume                     11779(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            14002
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.426
_diffrn_reflns_theta_min         1.357
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.758
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2950
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0700
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1900
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1916
_reflns_number_total             2950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc03190k2.cif
_cod_data_source_block           Zn-dbda
_cod_original_cell_volume        11778(3)
_cod_database_code               7119827
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.752
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C12-C13
 1.46 with sigma of 0.02
 C12_$1-C11_$1 = C13_$1-C10
 1.47 with sigma of 0.02
 C13_$1-C12_$1 = C13-C12
 1.51 with sigma of 0.01
 C11_$1-C10
 1.42 with sigma of 0.01
 C12_$1-C10
 2.08 with sigma of 0.02
 O3-C13_$1 = O4_$1-C12_$1 = O3_$1-C13 = O4-C12
 1.22 with sigma of 0.02
 N2-C10
 1.32 with sigma of 0.01
 C13_$2-C11_$2
 2.06 with sigma of 0.01
3. Restrained planarity
 C11_$2, C10_$3, C13_$2, C12_$2
 with sigma of 0.02
 C11_$1, C12_$1, C13_$1, C10, O3, O4_$1, N1_$1, N2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C4 \\sim C9: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C6 \\sim C5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C4 \\sim C9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C11 \\sim C10: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
O4 \\sim O3: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Others
 Fixed Sof: C2(0.5) C3(0.5) H3(0.5) C4(0.25) N2(0.25) C11(0.25) O3(0.25)
 N1(0.25) C9(0.25) C8(0.5) H8(0.5) C7(0.5) C6(0.25) H6(0.25) C5(0.25) H5(0.25)
 C10(0.25) C13(0.25) C12(0.25) O4(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C6(H6), C5(H5)
;
_shelx_res_checksum              91396
_shelx_hkl_checksum              49660
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'