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_1550671
_publ_section_title
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 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(C384 H208 B48 O320 Zr48)'
_chemical_formula_sum            'C24 H13 B3 O20 Zr3'
_chemical_formula_weight         927.43
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d'
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-23
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   40.5746(8)
_cell_length_b                   40.5746(8)
_cell_length_c                   17.0198(4)
_cell_measurement_reflns_used    3288
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      62.6430
_cell_measurement_theta_min      4.1440
_cell_volume                     28019.7(10)
_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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -108.00 -82.00   1.00   30.00    --  -42.06-138.00-103.00   26
  2  \w    -96.00  -2.00   1.00   30.00    --  -42.06 125.00 -90.00   94
  3  \w    102.00 128.00   1.00   60.00    --  107.13 125.00 150.00   26
  4  \w    113.00 178.00   1.00   60.00    --  107.13 125.00 -90.00   65
  5  \w     97.00 140.00   1.00   60.00    --  107.13 125.00-120.00   43
  6  \w     87.00 167.00   1.00   60.00    --  107.13  45.00 -30.00   80
;
_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      0.0139905000
_diffrn_orient_matrix_UB_12      -0.0115258000
_diffrn_orient_matrix_UB_13      0.0795330000
_diffrn_orient_matrix_UB_21      0.0035827000
_diffrn_orient_matrix_UB_22      0.0361623000
_diffrn_orient_matrix_UB_23      0.0262934000
_diffrn_orient_matrix_UB_31      -0.0351138000
_diffrn_orient_matrix_UB_32      -0.0009519000
_diffrn_orient_matrix_UB_33      0.0343121000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26464
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.581
_diffrn_reflns_theta_max         66.581
_diffrn_reflns_theta_min         3.560
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75646
_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            'dark colourless'
_exptl_crystal_density_diffrn    0.879
_exptl_crystal_description       block
_exptl_crystal_F_000             7232
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.153
_refine_diff_density_min         -2.398
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6381
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.1028
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2872
_refine_ls_wR_factor_ref         0.3466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3714
_reflns_number_total             6381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-108(Zr)
_cod_original_cell_volume        28019.7(13)
_cod_database_code               1550671
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.797
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O9(0.5) C8(0.5) C10(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C13(H13), C4(H4), C12(H12), C9(H9)
;
_shelx_res_checksum              88534
_shelx_fab_checksum              33476
_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 1.477
_oxdiff_exptl_absorpt_empirical_full_min 0.579