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_4125935
_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         'C144 H64 F12 O32 Zr6'
_chemical_formula_sum            'C144 H64 F12 O32 Zr6'
_chemical_formula_weight         3081.27
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.8364(2)
_cell_length_b                   39.8364(2)
_cell_length_c                   39.8364(2)
_cell_measurement_reflns_used    17849
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5420
_cell_measurement_theta_min      2.2470
_cell_volume                     63217.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_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 plate'
_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 0.998
_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   -110.00  27.00   1.00  120.00    --  -20.00 -18.00-180.00  137
  2  \w    -59.00  40.00   1.00  120.00    --  -20.00  54.00 -30.00   99
  3  \w    -36.00 -16.00   1.00  120.00    --  -20.00 -54.00-180.00   20
  4  \w   -108.00 -67.00   1.00  120.00    --  -20.00 -72.00-120.00   41
;
_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 MicroMesh'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0084456000
_diffrn_orient_matrix_UB_12      -0.0035941000
_diffrn_orient_matrix_UB_13      0.0152508000
_diffrn_orient_matrix_UB_21      -0.0142721000
_diffrn_orient_matrix_UB_22      -0.0089591000
_diffrn_orient_matrix_UB_23      0.0057741000
_diffrn_orient_matrix_UB_31      0.0064911000
_diffrn_orient_matrix_UB_32      -0.0149614000
_diffrn_orient_matrix_UB_33      -0.0071378000
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            94790
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.771
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82643
_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_density_diffrn    0.647
_exptl_crystal_description       Prism
_exptl_crystal_F_000             12256
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         3410
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+550.9291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2807
_reflns_number_total             3410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02184_si_013.cif
_cod_data_source_block           Zr-L3
_cod_depositor_comments
'Adding full bibliography for 4125932--4125938.cif.'
_cod_original_cell_volume        63217.9(10)
_cod_database_code               4125935
_chemical_oxdiff_formula         Zr6O4(OH4)(C24H10O4F2)6
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Zr1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: F1(0.5) H9(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9)
;
_shelx_res_checksum              84094
_shelx_hkl_checksum              51457
_shelx_fab_checksum              50186
_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 1.999
_oxdiff_exptl_absorpt_empirical_full_min 0.520