Single-Crystal to Single-Crystal Mechanical Contraction of Metal-Organic Frameworks through Stereoselective Postsynthetic Bromination.
Marshall, Ross J.; Griffin, Sarah L.; Wilson, Claire; Forgan, Ross S.; Journal of the American Chemical Society 137 (2015) 9527–9530; doi:10.1021/jacs.5b05434

data_4124176
_publ_section_title
;
 Single-Crystal to Single-Crystal Mechanical Contraction of Metal-Organic
 Frameworks through Stereoselective Postsynthetic Bromination.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9527
_journal_page_last               9530
_journal_paper_doi               10.1021/jacs.5b05434
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'Hf6 O4(OH)4 (C16H8O4)6'
_chemical_formula_sum            'C96 H52 Hf6 O32'
_chemical_formula_weight         2788.31
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_cell_length_c                   30.1107(12)
_cell_measurement_reflns_used    21604
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_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_collection
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CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
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CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
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_computing_structure_solution
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
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_diffrn_ambient_temperature      100
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_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 225
               Slice: -39.5000 - 73.0000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 40.0000
                 Phi: -17.0000
                 XTD: 44.9831
              2theta: -17.1677
scan:
    Number of images: 61
               Slice: -65.0000 - -34.5000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 24.0000
                 Phi: 16.0000
                 XTD: 44.9831
              2theta: -17.1677
;
_diffrn_measurement_device       'four-circle \k diffractometer'
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_diffrn_measurement_method       'profile data from \w-scans'
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_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.019115
_diffrn_orient_matrix_UB_12      0.027009
_diffrn_orient_matrix_UB_13      0.002840
_diffrn_orient_matrix_UB_21      0.026798
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_diffrn_orient_matrix_UB_23      -0.003390
_diffrn_orient_matrix_UB_31      -0.004410
_diffrn_orient_matrix_UB_32      0.000341
_diffrn_orient_matrix_UB_33      -0.032915
_diffrn_radiation_monochromator  Mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            23032
_diffrn_reflns_point_group_measured_fraction_full 0.995
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         2.343
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.300
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.678
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Block
_exptl_crystal_F_000             5264
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.908
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         1601
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+190.3025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1495
_reflns_number_total             1601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05434_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4124172--4124178.cif.
;
_cod_original_cell_volume        27300(3)
_cod_database_code               4124176
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-C2
 1.48 with sigma of 0.01
 C3-C2 = C4-C3 = C5-C4
 1.39 with sigma of 0.01
 C6-C5
 1.434 with sigma of 0.02
 C6-C6_$1
 1.181 with sigma of 0.02
 C2-C4 \\sim C3-C5
 with sigma of 0.02
3. Restrained planarity
 C2, C3, C4, C5
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_checksum              35029
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_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20