Furnishing Amine-Functionalized Metal-Organic Frameworks with the β-Amidoketone Group by Postsynthetic Modification.
Gee, William J.; Cadman, Laura K.; Amer Hamzah, Harina; Mahon, Mary F.; Raithby, Paul R.; Burrows, Andrew D.; Inorganic chemistry 55 (2016) 10839–10842; doi:10.1021/acs.inorgchem.6b01917

data_4349124
_publ_section_title
;
 Furnishing Amine-Functionalized Metal-Organic Frameworks with the
 \b-Amidoketone Group by Postsynthetic Modification.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10839
_journal_page_last               10842
_journal_paper_doi               10.1021/acs.inorgchem.6b01917
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C6.16 H1.25 N0.75 O2.44 Zn0.5'
_chemical_formula_sum            'C7.13 H7.88 N O2.69 Zn0.5'
_chemical_formula_weight         183.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date
;
'Thu Jul 09 10:24:15 2015'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.526(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9532(6)
_cell_length_b                   16.6496(5)
_cell_length_c                   9.5586(3)
_cell_measurement_reflns_used    5188
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.6380
_cell_measurement_theta_min      4.7390
_cell_volume                     2183.24(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10650
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         70.074
_diffrn_reflns_theta_min         4.705
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       block
_exptl_crystal_F_000             753
_exptl_crystal_size_max          0.1786
_exptl_crystal_size_mid          0.1136
_exptl_crystal_size_min          0.0876
_refine_diff_density_max         1.705
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2151
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0890
_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^)+(0.1645P)^2^+13.0017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2045
_reflns_number_total             2151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01917_si_002.cif
_cod_data_source_block           s15prr65
_cod_original_cell_volume        2183.25(13)
_cod_original_formula_sum        'C7.13 H7.88 N O2.69 Zn0.50'
_cod_database_code               4349124
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C5-C6 \\sim N2-C5
 with sigma of 0.02
 O4-C7 \\sim O3-C5
 with sigma of 0.02
 C6-C7 \\sim C5-C6
 with sigma of 0.02
3. Restrained planarity
 O3, N2, C1, C2, C3, C4, C5
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N2) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
: with sigma of 0.03 and sigma for terminal atoms of 0.005
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.007
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O3(0.22) O4(0.22) N2(0.25) H2(0.25) C5(0.22) C6(0.22) C7(0.22)
 C8(0.25) C9(0.5) C11(0.25) C10(0.5)
 Fixed Uiso: O4(0.15) C7(0.15)
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4)
;
_shelx_fab_checksum              64568
_olex2_submission_special_instructions 'No special instructions were received'