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_1550673
_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(C640 H368 Cd28 N32 O192)'
_chemical_formula_sum            'C160 H96 Cd7 N8 O48'
_chemical_formula_weight         3685.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-16
_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                 105.239(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.872(2)
_cell_length_b                   19.2171(7)
_cell_length_c                   32.400(3)
_cell_measurement_reflns_used    4236
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      54.1240
_cell_measurement_theta_min      3.6010
_cell_volume                     19748(2)
_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      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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -102.00 -22.00   1.00   15.00    --  -41.81 -38.00-180.00   80
  2  \w   -116.00 -20.00   1.00   15.00    --  -41.81 -38.00 -60.00   96
  3  \w      4.00  45.00   1.00   15.00    --   41.81 -99.00  90.00   41
  4  \w     36.00  66.00   1.00   15.00    --   41.81-125.00-150.00   30
  5  \w     81.00 126.00   1.00   40.00    --  107.13  45.00  90.00   45
  6  \w    148.00 177.00   1.00   40.00    --  107.13  30.00  60.00   29
  7  \w    100.00 126.00   1.00   40.00    --  107.13 -61.00-150.00   26
  8  \w     42.00  69.00   1.00   40.00    --  107.13-125.00  90.00   27
  9  \w     92.00 121.00   1.00   40.00    --  107.13-125.00  90.00   29
 10  \w     39.00 110.00   1.00   40.00    --  107.13-125.00 -30.00   71
 11  \w     36.00  71.00   1.00   40.00    --  107.13 -61.00-150.00   35
 12  \w     78.00 178.00   1.00   40.00    --  107.13  77.00 120.00  100
 13  \w     79.00 122.00   1.00   40.00    --  107.13  30.00  60.00   43
;
_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      0.0361255000
_diffrn_orient_matrix_UB_12      0.0331576000
_diffrn_orient_matrix_UB_13      -0.0153229000
_diffrn_orient_matrix_UB_21      0.0160837000
_diffrn_orient_matrix_UB_22      0.0363854000
_diffrn_orient_matrix_UB_23      0.0436198000
_diffrn_orient_matrix_UB_31      0.0281553000
_diffrn_orient_matrix_UB_32      -0.0633528000
_diffrn_orient_matrix_UB_33      0.0170293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            36069
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.996
_diffrn_reflns_theta_max         65.996
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64966
_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 yellow'
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             7328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.912
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         17166
_refine_ls_number_restraints     1059
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_gt           0.1068
_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^)+(0.1981P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2963
_refine_ls_wR_factor_ref         0.3422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7168
_reflns_number_total             17166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-106
_cod_original_cell_volume        19748(3)
_cod_database_code               1550673
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cd'
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.442
_reflns_odcompleteness_completeness 99.69
_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,H) groups
2. Restrained distances
 C12-N1 = C21-N2
 1.48 with sigma of 0.02
 C61-N4 = C50-N3
 1.48 with sigma of 0.02
 C58-C57
 1.48 with sigma of 0.02
 C58-O13 = C58-O14
 1.25 with sigma of 0.02
 C72-C71
 1.5 with sigma of 0.01
 C40-C37
 1.5 with sigma of 0.01
 C1-C2
 1.48 with sigma of 0.02
 C1-O1 = C1-O2
 1.26 with sigma of 0.02
 C30-C31
 1.48 with sigma of 0.02
 C31-O21 = C31-O22
 1.26 with sigma of 0.02
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(Cd2) \\sim Ueq, Uanis(Cd3) \\sim Ueq, Uanis(Cd5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Cd4(0.66667) Cd5(0.33333)
6.a Rotating group:
 O10(H10A,H10B)
6.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C28(H28), C9(H9), C64(H64), C26(H26), C51(H51), C62(H62), C76(H76),
 C81(H81), C24(H24), C69(H69), C49(H49), C33(H33), C4(H4), C66(H66), C46(H46),
 C13(H13), C47(H47), C22(H22), C29(H29), C55(H55), C44(H44), C38(H38), C7(H7),
 C60(H60), C73(H73), C43(H43), C11(H11), C15(H15), C36(H36), C6(H6), C74(H74),
 C77(H77), C39(H39), C20(H20), C56(H56), C70(H70), C80(H80), C3(H3), C19(H19),
 C35(H35), C59(H59), C32(H32), C16(H16)
;
_shelx_res_checksum              9811
_shelx_fab_checksum              74671
_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 0.732