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_1550667
_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         '0.25(C160 H88 N8 O64 Zr12)'
_chemical_formula_sum            'C40 H22 N2 O16 Zr3'
_chemical_formula_weight         1060.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-04 deposited with the CCDC.    2019-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.956(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.346(2)
_cell_length_b                   18.477(4)
_cell_length_c                   18.0998(12)
_cell_measurement_reflns_used    1568
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      68.4800
_cell_measurement_theta_min      4.4380
_cell_volume                     11805(3)
_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    'ShelXT (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
;
  1 omega  -45.00    0.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605   38.0000  -90.0000 45

  2 omega -114.00  -23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605  -57.0000  150.0000 91

  3 omega  -84.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605  125.0000  -90.0000 82

  4 omega   92.00  151.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759   45.0000  150.0000 59

  5 omega   33.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759 -125.0000    0.0000 84

  6 omega   53.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759   15.0000  -90.0000 123

  7 omega   23.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -94.0000  150.0000 86

  8 omega  132.00  160.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  125.0000  -30.0000 28

  9 omega   39.00  125.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -61.0000  -30.0000 86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0093288000
_diffrn_orient_matrix_UB_12      -0.0740417000
_diffrn_orient_matrix_UB_13      -0.0337216000
_diffrn_orient_matrix_UB_21      -0.0058862000
_diffrn_orient_matrix_UB_22      -0.0366931000
_diffrn_orient_matrix_UB_23      0.0749797000
_diffrn_orient_matrix_UB_31      -0.0422270000
_diffrn_orient_matrix_UB_32      -0.0112508000
_diffrn_orient_matrix_UB_33      -0.0223300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1807
_diffrn_reflns_av_unetI/netI     0.2013
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22058
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        62.991
_diffrn_reflns_theta_max         62.991
_diffrn_reflns_theta_min         3.408
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.362
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29262
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.597
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.506
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         9846
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.1305
_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^)+(0.1802P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3114
_refine_ls_wR_factor_ref         0.3681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3861
_reflns_number_total             9846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-104
_cod_database_code               1550667
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Zr'
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.749
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Zr1-O2_$1
 2.02 with sigma of 0.002
 Zr2-O2
 2.02 with sigma of 0.002
3. 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
4. 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
Uanis(Zr1) \\sim Ueq, Uanis(Zr2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0
Uanis(O5) = Uanis(O6)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C19(H19), C18(H18), C4(H4), C13(H13), C11(H11), C7(H7), C16(H16),
 C9(H9), C6(H6), C15(H15)
;
_shelx_res_checksum              88531
_shelx_fab_checksum              32660
_olex2_submission_special_instructions 'No special instructions were received'