Flexible metal‒organic frameworks for the wavelength-based luminescence sensing of aqueous pH
Lv, Xiu-Liang; Xie, Lin-Hua; Wang, Bin; Zhao, Minjian; Cui, Yuanjing; Li, Jian-Rong; Journal of Materials Chemistry C 6 (2018) 10628–; doi:10.1039/C8TC03036G

data_7237447
_publ_section_title
;
 Flexible metal--organic frameworks for the wavelength-based luminescence
 sensing of aqueous pH
;
_journal_issue                   39
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              10628
_journal_paper_doi               10.1039/C8TC03036G
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         '0.13(C328 H184 N8 O128 Zr24)'
_chemical_formula_sum            'C41 H23 N O16 Zr3'
_chemical_formula_weight         1059.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_Hall           '-I 2 2'
_space_group_name_H-M_alt        'I m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-02-17 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5401(6)
_cell_length_b                   33.1625(6)
_cell_length_c                   31.9996(9)
_cell_measurement_reflns_used    6364
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.6700
_cell_measurement_theta_min      3.6170
_cell_volume                     22858.1(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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    -96.00  -2.00   1.00   12.50    --  -41.81 125.00 -60.00   94
  2  \w     23.00  98.00   1.00   12.50    --   41.81-125.00 150.00   75
  3  \w      1.00  79.00   1.00   12.50    --   41.81 -99.00 -90.00   78
  4  \w     80.00 177.00   1.00   35.00    --  105.88  77.00-120.00   97
  5  \w     38.00  64.00   1.00   35.00    --  105.88 -45.00-120.00   26
  6  \w     79.00 131.00   1.00   35.00    --  105.88 -45.00-120.00   52
  7  \w    139.00 173.00   1.00   35.00    --  105.88 125.00-120.00   34
  8  \w     99.00 126.00   1.00   35.00    --  105.88 125.00 -60.00   27
  9  \w     51.00 100.00   1.00   35.00    --  105.88-125.00  60.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0375632000
_diffrn_orient_matrix_UB_12      0.0031008000
_diffrn_orient_matrix_UB_13      -0.0409118000
_diffrn_orient_matrix_UB_21      -0.0295050000
_diffrn_orient_matrix_UB_22      -0.0396371000
_diffrn_orient_matrix_UB_23      -0.0154217000
_diffrn_orient_matrix_UB_31      -0.0531780000
_diffrn_orient_matrix_UB_32      0.0240418000
_diffrn_orient_matrix_UB_33      -0.0202084000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            36277
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.939
_diffrn_reflns_theta_min         3.637
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         11951
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0625P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7534
_reflns_number_total             11951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc03036g4.cif
_cod_data_source_block           exp_481
_cod_database_code               7237447
_chemical_oxdiff_formula         'C H O N Zr'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Uiso/Uaniso restraints and constraints
O7 \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H14C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C11(H11), C16(H16), C17(H17),
 C19(H19), C20(H20)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              51021
_shelx_shelxl_version_number     2016/6
_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 1.578
_oxdiff_exptl_absorpt_empirical_full_min 0.801