Functional Versatility of a Series of Zr Metal-Organic Frameworks Probed by Solid-State Photoluminescence Spectroscopy.
Marshall, Ross J.; Kalinovskyy, Yaroslav; Griffin, Sarah L.; Wilson, Claire; Blight, Barry A.; Forgan, Ross S.; Journal of the American Chemical Society 139 (2017) 6253–6260; doi:10.1021/jacs.7b02184

data_4125933
_publ_section_title
;
 Functional Versatility of a Series of Zr Metal-Organic Frameworks Probed
 by Solid-State Photoluminescence Spectroscopy.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6253
_journal_page_last               6260
_journal_paper_doi               10.1021/jacs.7b02184
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'Zr6 O4 (OH)4 (C28 H14 O4)6'
_chemical_formula_sum            'C168 H88 O32 Zr6'
_chemical_formula_weight         3165.70
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m'
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.8785(3)
_cell_length_b                   39.8785(3)
_cell_length_c                   39.8785(3)
_cell_measurement_reflns_used    14130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2710
_cell_measurement_theta_min      2.0510
_cell_volume                     63418.6(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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   -109.00  20.00   0.50  110.00    --  -19.00 -54.00 114.00  258
  2  \w    -79.00  13.50   0.50  110.00    --  -19.00 -54.00 -17.00  185
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0163812000
_diffrn_orient_matrix_UB_12      -0.0045026000
_diffrn_orient_matrix_UB_13      -0.0052618000
_diffrn_orient_matrix_UB_21      -0.0056350000
_diffrn_orient_matrix_UB_22      -0.0008120000
_diffrn_orient_matrix_UB_23      -0.0168523000
_diffrn_orient_matrix_UB_31      0.0040333000
_diffrn_orient_matrix_UB_32      0.0171866000
_diffrn_orient_matrix_UB_33      -0.0021713000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1666
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            73411
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         1.769
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    0.663
_exptl_crystal_description       prism
_exptl_crystal_F_000             12736
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0744
_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^)+(0.1298P)^2^+250.3695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2274
_reflns_number_total             3415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02184_si_016.cif
_cod_data_source_block           Zr-L6
_cod_depositor_comments
'Adding full bibliography for 4125932--4125938.cif.'
_cod_original_cell_volume        63418.6(16)
_cod_database_code               4125933
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.41
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6
 1.181 with sigma of 0.02
 C6-C5 = C8-C7
 1.434 with sigma of 0.02
 C3-C2 = C4-C3 = C5-C4 = C9-C8 = C9-C10 = C11-C10 = C11-C11_$1 = C8-C12_$2 =
 C12_$2-C12_$3 = C9-C9_$1
 1.39 with sigma of 0.01
 C3-C3_$2 \\sim C2-C4 \\sim C9-C11 \\sim C10-C11_$1 \\sim C9_$1-C12_$3
 with sigma of 0.02
3. Restrained planarity
 C8, C9, C10, C11, C11_$1, C10_$1, C9_$1, C8_$3, C12_$3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C12 \\sim C9 \\sim C10 \\sim C11: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Others
 Fixed Sof: C9(0.5) C10(0.5) C11(0.5) H11(0.5) C12(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C11(H11)
;
_shelx_res_checksum              11870
_shelx_hkl_checksum              70088
_shelx_fab_checksum              82355
_shelx_shelxl_version_number     2014/7
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.882