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_1550674
_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         'C40 H22 In N2 O8'
_chemical_formula_sum            'C40 H22 In N2 O8'
_chemical_formula_weight         773.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-21
_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                90
_cell_formula_units_Z            8
_cell_length_a                   32.0315(3)
_cell_length_b                   28.2049(3)
_cell_length_c                   19.8600(2)
_cell_measurement_reflns_used    22196
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      66.1650
_cell_measurement_theta_min      2.6260
_cell_volume                     17942.4(3)
_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      243(2)
_diffrn_detector                 'CCD plate'
_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     42.00  67.20   0.40    1.00    --    5.00  32.00-174.00   63
  2  \w    -32.00  -6.00   0.40    1.00    --  -45.20  32.00-174.00   65
  3  \w   -108.00 -82.00   0.40    1.00    --  -45.20 -32.00  26.00   65
  4  \w    -87.00 -61.00   0.40   20.00    -- -100.10  32.00-174.00   65
  5  \w   -163.00-137.00   0.40   20.00    -- -100.10 -32.00  26.00   65
  6  \w     -8.00  90.00   0.40    1.00    --    5.00  57.00  30.00  245
  7  \w   -130.00 -34.00   0.40    1.00    --  -45.20 -38.00 -60.00  240
  8  \w   -112.00 -70.00   0.40    1.00    --  -45.20 -72.00 -90.00  105
  9  \w   -117.00 -89.00   0.40   20.00    -- -100.10 -19.00 -30.00   70
 10  \w   -187.00 -89.00   0.40   20.00    -- -100.10 -72.00 -60.00  245
 11  \w   -114.00 -32.00   0.40   20.00    -- -100.10  72.00  30.00  205
 12  \w   -185.00 -97.00   0.40   20.00    -- -100.10 -19.00  60.00  220
 13  \w   -169.00-119.80   0.40   20.00    -- -100.10 -19.00 -30.00  123
 14  \w    -47.00 -21.00   0.40   20.00    -- -100.10  72.00-150.00   65
 15  \w   -106.00 -14.80   0.40   20.00    -- -100.10  57.00 -60.00  228
;
_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      0.0026852000
_diffrn_orient_matrix_UB_12      0.0541606000
_diffrn_orient_matrix_UB_13      0.0085864000
_diffrn_orient_matrix_UB_21      -0.0439016000
_diffrn_orient_matrix_UB_22      0.0052362000
_diffrn_orient_matrix_UB_23      -0.0307307000
_diffrn_orient_matrix_UB_31      -0.0194890000
_diffrn_orient_matrix_UB_32      -0.0043418000
_diffrn_orient_matrix_UB_33      0.0707358000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79338
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.596
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         2.618
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85832
_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 gold'
_exptl_crystal_density_diffrn    0.573
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         15832
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0706
_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^)+(0.1672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2197
_refine_ls_wR_factor_ref         0.2308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11575
_reflns_number_total             15832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-107
_cod_database_code               1550674
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'In C N O'
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.683
_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. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C32(H32), C18(H18), C39(H39), C40(H40), C33(H33), C26(H26),
 C29(H29), C19(H19), C13(H13), C28(H28), C16(H16), C35(H35), C22(H22), C36(H36),
  C15(H15), C11(H11), C3(H3), C4(H4), C9(H9), C7(H7), C6(H6)
;
_shelx_res_checksum              16243
_shelx_fab_checksum              87661
_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 1.357
_oxdiff_exptl_absorpt_empirical_full_min 0.818