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_1550666
_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         '0.06(C252 H162 Cu18 N18 O72)'
_chemical_formula_sum            'C14 H9 Cu N O4'
_chemical_formula_weight         318.76
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2017-11-14
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-01-04 deposited with the CCDC.    2019-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   18.6355(7)
_cell_length_b                   18.6355(7)
_cell_length_c                   34.4019(12)
_cell_measurement_reflns_used    3995
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      74.2420
_cell_measurement_theta_min      3.7200
_cell_volume                     10346.5(7)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_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    -70.00  20.00   1.00    3.00    --  -41.94  57.00 -90.00   90
  2  \w      6.00  36.00   1.00    3.00    --   41.94 -38.00 -60.00   30
  3  \w    145.00 175.00   1.00   10.00    --  107.13 125.00 -60.00   30
  4  \w     84.00 177.00   1.00   10.00    --  107.13  45.00 120.00   93
  5  \w     95.00 157.00   1.00   10.00    --  107.13 125.00 120.00   62
  6  \w     36.00 104.00   1.00   10.00    --  107.13 -61.00  60.00   68
;
_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      0.0066536000
_diffrn_orient_matrix_UB_12      0.0013675000
_diffrn_orient_matrix_UB_13      -0.0446060000
_diffrn_orient_matrix_UB_21      -0.0942962000
_diffrn_orient_matrix_UB_22      -0.0355188000
_diffrn_orient_matrix_UB_23      -0.0032414000
_diffrn_orient_matrix_UB_31      0.0134318000
_diffrn_orient_matrix_UB_32      0.0886175000
_diffrn_orient_matrix_UB_33      -0.0006567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            7625
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.756
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65582
_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            'light green'
_exptl_crystal_density_diffrn    0.921
_exptl_crystal_description       block
_exptl_crystal_F_000             2898
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0750P)^2^+16.2290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2064
_reflns_number_total             2276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-101(Cu)
_cod_original_cell_volume        10346.5(9)
_cod_database_code               1550666
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O N Cu'
_reflns_odcompleteness_completeness 99.96
_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
2. Others
 Fixed Sof: H00A(0.5) H00B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 N004(H00A,H00B)
3.b Aromatic/amide H refined with riding coordinates:
 C007(H007), C00A(H00C), C00C(H00D), C00D(H00E)
;
_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 1.320
_oxdiff_exptl_absorpt_empirical_full_min 0.799