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_1550675
_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(C1440 H792 N72 O432 Zn90)'
_chemical_formula_sum            'C80 H44 N4 O24 Zn5'
_chemical_formula_weight         1772.04
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-19
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   54.3601(10)
_cell_length_b                   54.3601(10)
_cell_length_c                   42.0659(13)
_cell_measurement_reflns_used    8546
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      47.2140
_cell_measurement_theta_min      2.3630
_cell_volume                     107652(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -56.00   1.05   0.35   20.00    --  -45.20  71.00  85.00  163
  2  \w   -177.00 -97.90   0.35   60.00    -- -100.10 -71.00 -44.00  226
  3  \w   -181.00-107.15   0.35   60.00    -- -100.10 -59.00-103.00  211
  4  \w   -120.00 -35.30   0.35   20.00    --  -45.20 -19.00   0.00  242
  5  \w   -168.00 -95.90   0.35   60.00    -- -100.10 -57.00-150.00  206
  6  \w   -113.00 -18.85   0.35   60.00    -- -100.10  57.00-180.00  269
  7  \w   -118.00 -93.50   0.35   60.00    -- -100.10 -38.00 -60.00   70
  8  \w   -100.00 -17.05   0.35   60.00    -- -100.10  72.00 -30.00  237
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0245149000
_diffrn_orient_matrix_UB_12      -0.0126348000
_diffrn_orient_matrix_UB_13      -0.0242570000
_diffrn_orient_matrix_UB_21      -0.0090295000
_diffrn_orient_matrix_UB_22      0.0214335000
_diffrn_orient_matrix_UB_23      0.0107339000
_diffrn_orient_matrix_UB_31      0.0197098000
_diffrn_orient_matrix_UB_32      0.0212543000
_diffrn_orient_matrix_UB_33      -0.0252391000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            116821
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.073
_diffrn_reflns_theta_max         65.073
_diffrn_reflns_theta_min         2.301
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    0.492
_exptl_crystal_description       block
_exptl_crystal_F_000             16092
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         20392
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0938
_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^)+(0.1500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2655
_refine_ls_wR_factor_ref         0.3082
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7124
_reflns_number_total             20392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-105
_cod_original_cell_volume        107652(5)
_cod_database_code               1550675
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn C H O N'
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.841
_reflns_odcompleteness_completeness 99.90
_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
 C1-O3
 1.24 with sigma of 0.02
 C1-O2
 1.24 with sigma of 0.01
 C21-N2
 1.45 with sigma of 0.01
 C10-N1
 1.48 with sigma of 0.01
 O2-O3
 2.2 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C35(H35), C28(H28), C13(H13), C32(H32), C36(H36), C22(H22),
 C29(H29), C40(H40), C3(H3), C16(H16), C20(H20), C15(H15), C19(H19), C9(H9),
 C39(H39), C26(H26), C4(H4), C11(H11), C31(H31), C6(H6), C7(H7)
;
_shelx_res_checksum              79434
_shelx_fab_checksum              27866
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.734
_oxdiff_exptl_absorpt_empirical_full_min 0.473