Amino functionalized Zn/Cd-metal-organic frameworks for selective CO<sub>2</sub> adsorption and Knoevenagel condensation reactions.
Zhai, Zhi-Wei; Yang, Shuang-Hua; Lv, Ya-Ru; Du, Chen-Xia; Li, Lin-Ke; Zang, Shuang-Quan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4007–4014; doi:10.1039/c9dt00391f

data_7049138
_publ_section_title
;
 Amino functionalized Zn/Cd-metal-organic frameworks for selective
 CO<sub>2</sub> adsorption and Knoevenagel condensation reactions.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4007
_journal_page_last               4014
_journal_paper_doi               10.1039/c9dt00391f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C22 H13 N5 O4 S2 Zn, C3 H7 N O'
_chemical_formula_sum            'C25 H20 N6 O5 S2 Zn'
_chemical_formula_weight         613.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-17 deposited with the CCDC.    2019-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.5564(2)
_cell_length_b                   17.2237(2)
_cell_length_c                   16.5743(2)
_cell_measurement_reflns_used    8159
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5240
_cell_measurement_theta_min      3.5300
_cell_volume                     5297.31(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  89.00   0.50    0.50    --    0.00  19.00 -90.00  222
  2  \w     27.00  52.00   0.50    0.50    --    0.00  38.00  30.00   50
  3  \w     28.00  54.00   0.50    0.50    --    0.00  38.00 -60.00   52
  4  \w     53.00 123.00   0.50    2.50    --   95.20 -15.00   0.00  140
  5  \w     58.00 112.00   0.50    2.50    --   95.20 -30.00 -60.00  108
  6  \w     96.00 127.00   0.50    2.50    --   95.20  77.00 -60.00   62
  7  \w    142.00 169.00   0.50    2.50    --   95.20  77.00 -60.00   54
  8  \w     28.00 107.00   0.50    2.50    --   95.20 -30.00  30.00  158
  9  \w     36.00 124.00   0.50    2.50    --   95.20 -82.00 -90.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0558150000
_diffrn_orient_matrix_UB_12      0.0599457000
_diffrn_orient_matrix_UB_13      -0.0290847000
_diffrn_orient_matrix_UB_21      0.0340381000
_diffrn_orient_matrix_UB_22      0.0616750000
_diffrn_orient_matrix_UB_23      0.0554976000
_diffrn_orient_matrix_UB_31      0.0511824000
_diffrn_orient_matrix_UB_32      0.0244814000
_diffrn_orient_matrix_UB_33      -0.0686736000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18626
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.112
_diffrn_reflns_theta_min         3.501
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.179
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       needle
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5234
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+4.6588P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4601
_reflns_number_total             5234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00391f2.cif
_cod_data_source_block           20170629e1
_cod_depositor_comments
'Adding full bibliography for 7049138--7049139.cif.'
_cod_database_code               7049138
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N S Zn'
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.742
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C3A, C3B}
{C4A, C4B}
3. Restrained distances
 O6A-C26 \\sim O6B-C26
 with sigma of 0.01
 N7-C27B \\sim N7-C27A \\sim N7-C28B \\sim N7-C28A \\sim N7-C26
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C27A \\sim C28A \\sim C27B \\sim C28B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28A) \\sim Ueq, Uanis(C28B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3A) = Uanis(C3B)
Uanis(C4A) = Uanis(C4B)
5. Others
 Fixed Sof: C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C23(0.5) H23(0.5) C24(0.5)
 H24A(0.5) H24B(0.5) H24C(0.5) C26(0.5) H26(0.25) H26A(0.25) O6A(0.25) N5A(0.5)
 H5AA(0.5) H5AB(0.5) C27A(0.25) H27A(0.25) H27B(0.25) H27C(0.25) C3A(0.5)
 C4B(0.5) H4B(0.5) C28A(0.25) H28A(0.25) H28B(0.25) H28C(0.25) O6B(0.25)
 N5B(0.5) H5BA(0.5) H5BB(0.5) C27B(0.25) H27D(0.25) H27E(0.25) H27F(0.25)
 C4A(0.5) C3B(0.5) H3B(0.5) C28B(0.25) H28D(0.25) H28E(0.25) H28F(0.25)
6.a Riding coordinates:
 C24(H24A,H24B,H24C), C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C27B(H27D,
 H27E,H27F), C28B(H28D,H28E,H28F)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C20(H20), C13(H13), C10(H10), C6(H6), C23(H23), C21(H21), C22(H22),
 C26(H26), C26(H26A), C12(H12), C7(H7), C19(H19), C4B(H4B), C3B(H3B)
6.c X=CH2 refined with riding coordinates:
 N5A(H5AA,H5AB), N5B(H5BA,H5BB)
6.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              82771
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.301
_oxdiff_exptl_absorpt_empirical_full_min 0.716