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_4124177
_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         'Zr6O4(OH)4 (C16H8O4Br2)6'
_chemical_formula_sum            'C96 H52 Br12 O32 Zr6'
_chemical_formula_weight         3223.61
_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             2015-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.861(2)
_cell_length_b                   29.861(2)
_cell_length_c                   29.861(2)
_cell_measurement_reflns_used    18323
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     26626(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_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_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
    Number of images: 118
               Slice: -45.0000 - 73.0000
         Image width: 1.0000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 24.0000
                 Phi: -82.0000
                 XTD: 45.0264
              2theta: -17.2610
scan:
    Number of images: 26
               Slice: -51.0000 - -25.0000
         Image width: 1.0000
            Exp time: 30.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 40.0000
                 Phi: -82.0000
                 XTD: 45.0264
              2theta: -17.2610
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.006514
_diffrn_orient_matrix_UB_12      -0.032822
_diffrn_orient_matrix_UB_13      -0.001313
_diffrn_orient_matrix_UB_21      -0.027612
_diffrn_orient_matrix_UB_22      -0.004747
_diffrn_orient_matrix_UB_23      -0.018344
_diffrn_orient_matrix_UB_31      0.017793
_diffrn_orient_matrix_UB_32      0.004651
_diffrn_orient_matrix_UB_33      -0.027986
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_monochromator  Mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_laue_measured_fraction_full 0.993
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            22280
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.729
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.058
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.726
_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    0.804
_exptl_crystal_description       Block
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         1567
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0783
_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^)+(0.1089P)^2^+317.9326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1236
_reflns_number_total             1567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05434_si_002.cif
_cod_data_source_block           1BR2
_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        26626(5)
_cod_database_code               4124177
_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
 C3A-C2 = C4A-C3A = C5-C4A
 1.39 with sigma of 0.01
 C5-C6
 1.48 with sigma of 0.01
 Br1-C6
 1.88 with sigma of 0.02
 Br1-C6
 1.88 with sigma of 0.02
 C6-C6_$1
 1.32 with sigma of 0.02
3. Restrained planarity
 C2, C3A, C4A, C5
 with sigma of 0.1
4. Others
 Fixed Sof: Br1(0.25) C6(0.25) C4A(0.5) H4A(0.5) C3A(0.5) H3A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C3A(H3A)
;
_shelx_res_checksum              16146
_shelx_hkl_checksum              55972
_shelx_fab_checksum              5774
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'