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_1550668
_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(C384 H208 B48 Hf48 O320)'
_chemical_formula_sum            'C24 H13 B3 Hf3 O20'
_chemical_formula_weight         1189.24
_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
_atom_sites_solution_primary     dual
_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                   40.4997(4)
_cell_length_b                   40.4997(4)
_cell_length_c                   16.9534(4)
_cell_measurement_reflns_used    15582
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.6800
_cell_measurement_theta_min      4.1700
_cell_volume                     27807.4(8)
_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      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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    -16.00  49.00   0.50    2.00    --  -38.80  68.00 -86.00  130
  2  \w    -62.00 -25.00   0.50    2.00    --  -38.80  68.00 -86.00   74
  3  \w   -102.00 -70.00   0.50    2.00    --  -38.80 -52.00 -49.00   64
  4  \w   -161.00-136.00   0.50   12.00    -- -104.00 -52.00 -49.00   50
  5  \w    -75.00 -15.00   0.50   12.00    -- -104.00  68.00 -86.00  120
  6  \w   -160.00-135.00   0.50   12.00    -- -104.00 -68.00 140.00   50
  7  \w     13.00  38.00   0.50    2.00    --    5.00  68.00 -86.00   50
  8  \w      2.00  51.00   0.50    2.00    --    5.00  38.00-180.00   98
  9  \w   -125.00 -15.00   0.50   12.00    -- -104.00  72.00  30.00  220
 10  \w   -109.00 -84.00   0.50   12.00    -- -104.00 -38.00-180.00   50
 11  \w   -119.00 -86.00   0.50   12.00    -- -104.00  19.00  60.00   66
 12  \w    -79.00 -34.00   0.50   12.00    -- -104.00  19.00  60.00   90
 13  \w   -142.00-116.00   0.50   12.00    -- -104.00 -38.00-180.00   52
 14  \w   -180.00-154.00   0.50   12.00    -- -104.00 -38.00-180.00   52
 15  \w   -125.00 -28.00   0.50   12.00    -- -104.00  72.00 -30.00  194
 16  \w    -76.00 -51.00   0.50   12.00    -- -104.00  57.00-180.00   50
;
_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      -0.0263720000
_diffrn_orient_matrix_UB_12      -0.0163452000
_diffrn_orient_matrix_UB_13      0.0524548000
_diffrn_orient_matrix_UB_21      -0.0133771000
_diffrn_orient_matrix_UB_22      0.0343323000
_diffrn_orient_matrix_UB_23      0.0225405000
_diffrn_orient_matrix_UB_31      -0.0239121000
_diffrn_orient_matrix_UB_32      -0.0011437000
_diffrn_orient_matrix_UB_33      -0.0707023000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42600
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         3.571
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    8.422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58782
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             8768
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6304
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0593
_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^)+(0.1071P)^2^+124.6450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1742
_refine_ls_wR_factor_ref         0.1842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5212
_reflns_number_total             6304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00178f2.cif
_cod_data_source_block           BUT-108(Hf)
_cod_original_cell_volume        27807.4(9)
_cod_database_code               1550668
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O B Hf'
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.486
_reflns_odcompleteness_completeness 97.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C13-O4 = C13-O5
 1.4 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(C15) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Others
 Fixed Sof: C13(0.5) O11(0.5) C14(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C8(H8), C3(H3), C7(H7), C4(H4), C15(H15)
;
_shelx_res_checksum              74199
_shelx_fab_checksum              66032
_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 2.785
_oxdiff_exptl_absorpt_empirical_full_min 0.446