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_4126093
_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         'C24 H12 F2 O4, 2(C3 H7 N O)'
_chemical_formula_sum            'C30 H26 F2 N2 O6'
_chemical_formula_weight         548.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                74.409(3)
_cell_angle_beta                 74.790(3)
_cell_angle_gamma                75.265(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5707(3)
_cell_length_b                   11.0072(4)
_cell_length_c                   13.7230(5)
_cell_measurement_reflns_used    10976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5370
_cell_measurement_theta_min      2.2930
_cell_volume                     1317.16(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -95.00  24.00   1.00   10.00    --   -5.00 -72.00 -30.00  119
  2  \w    -29.00  85.00   1.00   10.00    --   -5.00  54.00  60.00  114
  3  \w    -60.00  12.00   1.00   10.00    --   -5.00 -54.00 120.00   72
  4  \w    -95.00  24.00   1.00   10.00    --   -5.00 -72.00   0.00  119
;
_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      -0.0385291000
_diffrn_orient_matrix_UB_12      -0.0143634000
_diffrn_orient_matrix_UB_13      -0.0318326000
_diffrn_orient_matrix_UB_21      -0.0022869000
_diffrn_orient_matrix_UB_22      -0.0615756000
_diffrn_orient_matrix_UB_23      0.0331118000
_diffrn_orient_matrix_UB_31      -0.0681833000
_diffrn_orient_matrix_UB_32      0.0256932000
_diffrn_orient_matrix_UB_33      0.0300067000
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22023
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         2.250
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90726
_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    1.383
_exptl_crystal_description       Plate
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0620P)^2^+0.3950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4437
_reflns_number_total             6070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02184_si_004.cif
_cod_data_source_block           L4-H2
_cod_original_cell_volume        1317.16(9)
_cod_database_code               4126093
_chemical_oxdiff_formula         'Hf4O6(OH)4(C24H10 O4F2)(C3H7NO)2'
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C20(H20), C14(H14), C6(H6), C23(H23), C7(H7), C19(H19), C22(H22),
 C27(H27), C3(H3A), C11(H11), C30(H30)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C26(H26A,H26B,
 H26C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3)
;
_shelx_res_checksum              32499
_shelx_hkl_checksum              53052
_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 1.514
_oxdiff_exptl_absorpt_empirical_full_min 0.784