Postsynthetic bromination of UiO-66 analogues: altering linker flexibility and mechanical compliance.
Marshall, Ross J.; Richards, Tom; Hobday, Claire L.; Murphie, Colin F.; Wilson, Claire; Moggach, Stephen A.; Bennett, Thomas D.; Forgan, Ross S.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 4132–4135; doi:10.1039/c5dt03178h

data_7038635
_publ_section_title
;
 Postsynthetic bromination of UiO-66 analogues: altering linker
 flexibility and mechanical compliance.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4132
_journal_page_last               4135
_journal_paper_doi               10.1039/c5dt03178h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         ' Zr6 O4 (O H)4 (C16 H10 O4 Br2)6'
_chemical_formula_sum            'C96 H64 Br12 O32 Zr6'
_chemical_formula_weight         3235.71
_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
_audit_creation_date             2015-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-14 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.7685(8)
_cell_length_b                   29.7685(8)
_cell_length_c                   29.7685(8)
_cell_measurement_reflns_used    12321
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     26379.8(12)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)'
_computing_data_reduction
'CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
    Number of images: 104
               Slice: -31.0000 - 73.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: 0.0000
                 XTD: 45.0166
              2theta: -17.2137
scan:
    Number of images: 91
               Slice: -69.0000 - 22.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -120.0000
                 XTD: 45.0166
              2theta: -17.2137
scan:
    Number of images: 93
               Slice: -71.0000 - 22.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 60.0000
                 XTD: 45.0166
              2theta: -17.2137
scan:
    Number of images: 84
               Slice: -59.0000 - 25.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: -150.0000
                 XTD: 45.0166
              2theta: -17.2137
scan:
    Number of images: 18
               Slice: -26.0000 - -8.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: -180.0000
                 XTD: 45.0166
              2theta: -17.2137
scan:
    Number of images: 108
               Slice: -35.0000 - 73.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 72.0000
                 Phi: 60.0000
                 XTD: 45.0166
              2theta: -17.2137
scan:
    Number of images: 100
               Slice: -78.0000 - 22.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: -60.0000
                 XTD: 45.0166
              2theta: -17.2137
scan:
    Number of images: 90
               Slice: -68.0000 - 22.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -72.0000
                 Phi: 120.0000
                 XTD: 45.0166
              2theta: -17.2137
scan:
    Number of images: 57
               Slice: -87.0000 - -30.0000
         Image width: 1.0000
            Exp time: 60.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: -60.0000
                 XTD: 45.0166
              2theta: -17.2137
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support MiTeGen
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.011322
_diffrn_orient_matrix_UB_12      0.031481
_diffrn_orient_matrix_UB_13      0.003037
_diffrn_orient_matrix_UB_21      -0.022204
_diffrn_orient_matrix_UB_22      -0.005614
_diffrn_orient_matrix_UB_23      -0.024575
_diffrn_orient_matrix_UB_31      -0.022522
_diffrn_orient_matrix_UB_32      -0.010290
_diffrn_orient_matrix_UB_33      0.022700
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            95174
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.987
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         2.737
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.077
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.815
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         1211
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0843
_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^)+(0.1770P)^2^+230.5540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2562
_refine_ls_wR_factor_ref         0.2677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1075
_reflns_number_total             1211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03178h2.cif
_cod_data_source_block           2Br2
_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/RSC/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 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        26380(2)
_cod_database_code               7038635
_platon_squeeze_void_probe_radius 1.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Br1-C6
 1.9 with sigma of 0.02
 C6-C6_$1
 1.53 with sigma of 0.02
 C6-C5
 1.5 with sigma of 0.02
 C3X-C2 = C4X-C3X = C5-C4X
 1.39 with sigma of 0.02
 Br1-C5 \\sim Br1-C6_$1
 with sigma of 0.02
3. Restrained planarity
 C2, C3X, C4X, C5
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C5 \\sim C6 \\sim C4X \\sim C3X: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
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. Others
 Fixed Sof: C6(0.25) C4X(0.5) H4X(0.5) C3X(0.5) H3X(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C4X(H4X), C3X(H3X)
;
_shelx_fab_checksum              24727
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'