Constructing New Metal-Organic Frameworks with Complicated Ligands Generated from “One-Pot” In Situ Reactions
Kong, Xiang-Jing; He, Tao; Zhang, Yongzheng; Wu, Xue-Qian; Wang, Si-Nan; Xu, Ming-Ming; Si, Guang-Rui; Li, Jian-Rong Jeff; Chemical Science  (2019) –; doi:10.1039/C9SC00178F

data_1550670
_publ_section_title
;
 Constructing New Metal-Organic Frameworks with Complicated Ligands
 Generated from &#x201C;One-Pot&#x201D; In Situ Reactions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00178F
_journal_year                    2019
_chemical_formula_moiety         'C14 H11 Cd N O5'
_chemical_formula_sum            'C14 H11 Cd N O5'
_chemical_formula_weight         385.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-01-04 deposited with the CCDC.    2019-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                87.203(3)
_cell_angle_beta                 74.302(3)
_cell_angle_gamma                76.159(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6897(3)
_cell_length_b                   8.7992(3)
_cell_length_c                   12.7198(4)
_cell_measurement_reflns_used    6264
_cell_measurement_temperature    292.5(4)
_cell_measurement_theta_max      73.8780
_cell_measurement_theta_min      5.1480
_cell_volume                     804.39(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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      air
_diffrn_ambient_temperature      292.5(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1688
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -66.00  32.00   1.00    1.00    --  -41.94  38.00 120.00   98
  2  \w   -116.00 -17.00   1.00    1.00    --  -41.94 -38.00  60.00   99
  3  \w    -75.00  34.00   1.00    1.00    --  -41.94  77.00 -30.00  109
  4  \w    -70.00  31.00   1.00    1.00    --  -41.94  57.00-150.00  101
  5  \w     24.00  99.00   1.00    1.00    --   41.94-126.00-121.00   75
  6  \w     35.00 136.00   1.00    1.00    --  107.13 -61.00 -30.00  101
  7  \w     31.00 140.00   1.00    1.00    --  107.13 -77.00 150.00  109
  8  \w     34.00 121.00   1.00    1.00    --  107.13-125.00  30.00   87
  9  \w     34.00 121.00   1.00    1.00    --  107.13-125.00 150.00   87
 10  \w     81.00 178.00   1.00    1.00    --  107.13  45.00 -30.00   97
 11  \w     78.00 178.00   1.00    1.00    --  107.13  61.00  30.00  100
 12  \w     31.00 140.00   1.00    1.00    --  107.13 -77.00-150.00  109
 13  \w     94.00 178.00   1.00    1.00    --  107.13 125.00-150.00   84
 14  \w     75.00 178.00   1.00    1.00    --  107.13  77.00 -90.00  103
 15  \w     81.00 178.00   1.00    1.00    --  107.13  45.00-150.00   97
 16  \w   -114.00 -14.00   1.00    1.00    --  -41.94 -57.00 -30.00  100
 17  \w   -114.00 -14.00   1.00    1.00    --  -41.94 -57.00 -90.00  100
 18  \w   -118.00  -9.00   1.00    1.00    --  -41.94 -77.00 120.00  109
 19  \w   -118.00  -9.00   1.00    1.00    --  -41.94 -77.00-150.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1469301000
_diffrn_orient_matrix_UB_12      -0.0837034000
_diffrn_orient_matrix_UB_13      -0.0142093000
_diffrn_orient_matrix_UB_21      -0.0652665000
_diffrn_orient_matrix_UB_22      -0.0166689000
_diffrn_orient_matrix_UB_23      0.1247618000
_diffrn_orient_matrix_UB_31      -0.1413901000
_diffrn_orient_matrix_UB_32      0.1588671000
_diffrn_orient_matrix_UB_33      0.0080372000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8628
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.052
_diffrn_reflns_theta_max         67.052
_diffrn_reflns_theta_min         3.610
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2643
_reflns_number_total             2871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-102
_cod_database_code               1550670
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 100.00
_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 N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1C,H1D)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C11(H11), C14(H14), C10(H10), C13(H13)
;
_shelx_res_checksum              35130
_shelx_fab_checksum              34461
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.898
_oxdiff_exptl_absorpt_empirical_full_min 0.690