Postsynthetic ionization of an imidazole-containing metal-organic framework for the cycloaddition of carbon dioxide and epoxides.
Liang, Jun; Chen, Rui-Ping; Wang, Xiu-Yun; Liu, Tao-Tao; Wang, Xu-Sheng; Huang, Yuan-Biao; Cao, Rong; Chemical science 8 (2017) 1570–1575; doi:10.1039/c6sc04357g

data_1544458
_publ_section_title
;
 Postsynthetic ionization of an imidazole-containing metal-organic
 framework for the cycloaddition of carbon dioxide and epoxides.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              1570
_journal_page_last               1575
_journal_paper_doi               10.1039/c6sc04357g
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C11 H9 N2 O4, Cl, H2 O'
_chemical_formula_sum            'C11 H11 Cl N2 O5'
_chemical_formula_weight         286.67
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-13 deposited with the CCDC.
2016-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9679(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.98145(13)
_cell_length_b                   21.3099(4)
_cell_length_c                   8.10016(14)
_cell_measurement_reflns_used    2831
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      73.2540
_cell_measurement_theta_min      5.5140
_cell_volume                     1193.46(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega  -50.00   36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1492   38.0000  120.0000 86

  2 omega   15.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1492  -99.0000   30.0000 31

  3 omega   34.00   94.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -45.0000  120.0000 60

  4 omega   42.00   85.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -45.0000   60.0000 43

  5 omega   45.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -30.0000  150.0000 31

  6 omega   33.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -30.0000    0.0000 57

  7 omega   30.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -30.0000  -60.0000 60

  8 omega   40.00  134.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -77.0000 -120.0000 94

  9 omega   59.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.1492 -125.0000 -120.0000 34

 10 omega   36.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -30.0000 -120.0000 52

 11 omega  -50.00   19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.1492   77.0000 -180.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1422291000
_diffrn_orient_matrix_UB_12      -0.0462194000
_diffrn_orient_matrix_UB_13      0.0985996000
_diffrn_orient_matrix_UB_21      0.1592343000
_diffrn_orient_matrix_UB_22      0.0505755000
_diffrn_orient_matrix_UB_23      0.0150366000
_diffrn_orient_matrix_UB_31      -0.0639600000
_diffrn_orient_matrix_UB_32      0.0231046000
_diffrn_orient_matrix_UB_33      0.1640106000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            4256
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.218
_diffrn_reflns_theta_min         4.149
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.051
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77014
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0419P)^2^+0.5619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2171
_reflns_number_total             2327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc04357g2.cif
_cod_data_source_block           exp_17348
_cod_depositor_comments
;Adding full bibliography for 1544458.cif.

 Adding full bibliography for 1544458.cif.
;
_cod_database_code               1544458
_chemical_oxdiff_formula         'N C H O Cl'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C10(H10), C11(H11)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
;
_shelx_res_checksum              20890
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'