A stable zinc‒organic framework with luminescence detection of acetylacetone in aqueous solution
Kang, Xiao-Min; Fan, Xi-Yu; Hao, Peng-Yuan; Wang, Wen-Min; Zhao, Bin; Inorganic Chemistry Frontiers 6 (2019) 271–; doi:10.1039/C8QI01260A

data_4349973
_publ_section_title
;
 A stable zinc--organic framework with luminescence detection of
 acetylacetone in aqueous solution
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              271
_journal_paper_doi               10.1039/C8QI01260A
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         '0.25(C224 H152 N32 O32 Zn8)'
_chemical_formula_sum            'C56 H38 N8 O8 Zn2'
_chemical_formula_weight         1081.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-05-11 deposited with the CCDC.
2018-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.226(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4791(7)
_cell_length_b                   12.9401(7)
_cell_length_c                   24.5733(14)
_cell_measurement_reflns_used    1708
_cell_measurement_temperature    120.8(2)
_cell_measurement_theta_max      27.2370
_cell_measurement_theta_min      3.3570
_cell_volume                     4883.0(4)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.8(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_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     20.00  86.00   1.00   35.00    --   18.94  77.00 -30.00   66
  2  \w     -1.00  88.00   1.00   35.00    --   18.94  57.00-150.00   89
  3  \w    -18.00   9.00   1.00   35.00    --  -19.25 -77.00-180.00   27
  4  \w     24.00  61.00   1.00   35.00    --   18.94 -99.00  60.00   37
  5  \w    -42.00 -10.00   1.00   35.00    --  -19.25  37.00 120.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0328892000
_diffrn_orient_matrix_UB_12      0.0379448000
_diffrn_orient_matrix_UB_13      -0.0008135000
_diffrn_orient_matrix_UB_21      0.0318284000
_diffrn_orient_matrix_UB_22      -0.0395537000
_diffrn_orient_matrix_UB_23      0.0004242000
_diffrn_orient_matrix_UB_31      -0.0062675000
_diffrn_orient_matrix_UB_32      -0.0015870000
_diffrn_orient_matrix_UB_33      -0.0290673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9965
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.952
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74232
_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    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0412P)^2^+2.5368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2879
_reflns_number_total             4299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi01260a2.cif
_cod_data_source_block           p151225b3_sq
_cod_database_code               4349973
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C Zn'
_chemical_oxdiff_usercomment     KXM-K27
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C15(H15), C7(H7), C6(H6), C5(H5), C14(H14), N3(H3A), C9(H9),
  C20(H20), C13(H13), C23(H23), C12(H12), C25(H25), C26(H26), C28(H28),
 C18(H18), C17(H17), C27(H27)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.621
_oxdiff_exptl_absorpt_empirical_full_min 0.635