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_4124175
_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         'Zr6 O4 (O H)4 (C16 H8 O4)6'
_chemical_formula_sum            'C96 H52 O32 Zr6'
_chemical_formula_weight         2264.69
_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                   30.2386(4)
_cell_length_b                   30.2386(4)
_cell_length_c                   30.2386(4)
_cell_measurement_reflns_used    20183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4600
_cell_measurement_theta_min      2.2110
_cell_volume                     27649.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)'
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -60.00   73.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000   14.0000   77.0000 133

  2 omega  -98.00   22.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -72.0000  128.0000 120

  3 omega  -82.00   22.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -72.0000  -78.0000 104

  4 omega  -38.00   -3.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -72.0000   25.0000 35

  5 omega   -1.00    9.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000  -44.0000  128.0000 10

  6 omega  -56.00   73.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000   72.0000 -129.0000 129

  7 omega  -74.00  -46.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0000   14.0000 -129.0000 28
;
_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_UB_11      0.0130359500
_diffrn_orient_matrix_UB_12      0.0168073500
_diffrn_orient_matrix_UB_13      0.0099151000
_diffrn_orient_matrix_UB_21      0.0042064000
_diffrn_orient_matrix_UB_22      0.0092195000
_diffrn_orient_matrix_UB_23      -0.0211488000
_diffrn_orient_matrix_UB_31      -0.0190490500
_diffrn_orient_matrix_UB_32      0.0135120500
_diffrn_orient_matrix_UB_33      0.0021165000
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_laue_measured_fraction_full 0.992
_diffrn_reflns_laue_measured_fraction_max 0.992
_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            77174
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.987
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         2.234
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    0.544
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             4496
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1264
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0686
_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^)+(0.0929P)^2^+166.5803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.1866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1171
_reflns_number_total             1264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b05434_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4124172--4124178.cif.'
_cod_original_cell_volume        27649.3(11)
_cod_database_code               4124175
_chemical_oxdiff_formula         'Zr6 O4 (O H)4 (C16 H12 O4)6'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.48
_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
 C3-C2 = C4-C3 = C5-C4
 1.39 with sigma of 0.02
 C3-C2 = C4-C3 = C5-C4
 1.39 with sigma of 0.02
 C6-C5
 1.434 with sigma of 0.02
 C6-C6_$1
 1.183 with sigma of 0.02
 C2-C4 \\sim C3-C5
 with sigma of 0.01
3. 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
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_checksum              85175
_shelx_hkl_checksum              74751
_shelx_fab_checksum              41480
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'