Reversible Multiphase Transition in a BioMOF and Its Distinctive Luminescence Turn-On in Alcohol Vapor.
Bai, Jian-Ping; Huang, Yong-Liang; Xie, Mo; Zhao, Yifang; Luo, Dong; Li, Yan Yan; Lu, Weigang; Li, Dan; ACS applied materials & interfaces 11 (2019) 38503–38509; doi:10.1021/acsami.9b14121

data_4514497
_publ_section_title
;
 Reversible Multiphase Transition in a BioMOF and Its Distinctive
 Luminescence Turn-On in Alcohol Vapor.
;
_journal_issue                   42
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              38503
_journal_page_last               38509
_journal_paper_doi               10.1021/acsami.9b14121
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety         '0.25(C444 H276.01 N104 O76 Zn32)'
_chemical_formula_sum            'C111 H69 N26 O19 Zn8'
_chemical_formula_weight         2593.88
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.346(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0332(5)
_cell_length_b                   23.8074(5)
_cell_length_c                   34.8396(8)
_cell_measurement_reflns_used    14547
_cell_measurement_temperature    100.00(15)
_cell_measurement_theta_max      76.4290
_cell_measurement_theta_min      2.7770
_cell_volume                     19770.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(15)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.952
_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    -28.00  33.00   0.50    7.50    --   -0.90 -82.00 -60.00  122
  2  \w    -31.00   2.00   0.50    7.50    --    0.90  82.00-180.00   66
  3  \w    -16.00  34.00   0.50    7.50    --    0.90 -82.00 120.00  100
  4  \w    -26.00  20.00   0.50    7.50    --    0.90  82.00  60.00   92
  5  \w     33.00  59.00   0.50   32.00    --  105.10 -77.00  30.00   52
  6  \w     82.00 170.00   0.50   32.00    --  105.10  82.00 -30.00  176
  7  \w     31.00 138.00   0.50   32.00    --  105.10 -77.00-120.00  214
  8  \w     56.00 106.00   0.50   32.00    --  105.10 -57.00-120.00  100
  9  \w     82.00 143.00   0.50   32.00    --  105.10  38.00 150.00  122
 10  \w    158.00 190.00   0.50   32.00    --  105.10  38.00 150.00   64
 11  \w     95.00 178.00   0.50   32.00    --  105.10  82.00  30.00  166
 12  \w     81.00 172.00   0.50   32.00    --  105.10  19.00 120.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0416064000
_diffrn_orient_matrix_UB_12      -0.0249973000
_diffrn_orient_matrix_UB_13      -0.0254876000
_diffrn_orient_matrix_UB_21      -0.0002394000
_diffrn_orient_matrix_UB_22      0.0556682000
_diffrn_orient_matrix_UB_23      -0.0226014000
_diffrn_orient_matrix_UB_31      0.0494354000
_diffrn_orient_matrix_UB_32      0.0215319000
_diffrn_orient_matrix_UB_33      0.0287761000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51263
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.992
_diffrn_reflns_theta_min         2.813
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.871
_exptl_crystal_description       block
_exptl_crystal_F_000             5236
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.646
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         20154
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0864
_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^)+(0.1815P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2396
_refine_ls_wR_factor_ref         0.2626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13273
_reflns_number_total             20154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b14121_si_001.cif
_cod_data_source_block           1_alfa
_cod_database_code               4514497
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.870
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: Zn4(0.3333) N0AA(0.5) C54(0.5) H54(0.5) N11(0.5) H11(0.5) C55(0.5)
 C56(0.5) N12(0.5) H12(0.5) C57(0.5) N13(0.5) H13A(0.5) H13B(0.5) N14(0.5)
 C58(0.5) N15(0.5) H15A(0.5) H15B(0.5) O11(0.3333) H11A(0.3333) H11B(0.3333)
 O12(0.667) H12A(0.667) H12B(0.667) Zn4A(0.667)
 Fixed U12: O1(0)
 Fixed U23: O1(0)
 Fixed Uiso: H1(0.055) H4A(0.108) H4B(0.108) H10(0.098) H19(0.11) H21(0.139)
 H25(0.099) H30(0.141) H32(0.111) H33(0.113) H34(0.123) H36(0.104) H37(0.111)
 H38(0.143) H40(0.134) H9A(0.166) H9B(0.166) H41(0.127) H42(0.152) H43(0.114)
 H44(0.139) H46(0.147) H47(0.128) H48(0.156) H49(0.119) H50(0.146) H51(0.163)
 H52(0.152) H53(0.17) H54(0.171) H11(0.221) H12(0.094) H13A(0.138) H13B(0.138)
 H15A(0.429) H15B(0.429) H11A(0.167) H11B(0.167) H12A(0.263) H12B(0.263)
 Fixed X: O1(0.5) H1(0.455963) H4A(0.59448) H4B(0.554759) H10(0.51996)
 H19(0.615106) H21(0.403375) H25(0.486204) H30(0.336962) H32(0.799179)
 H33(0.493951) H34(0.201148) H36(0.845023) H37(0.525149) H38(0.64129)
 H40(0.705076) H9A(0.648296) H9B(0.626233) H41(0.707294) H42(0.426907)
 H43(0.689503) H44(0.295649) H46(0.327698) H47(0.234429) H48(0.352323)
 H49(0.753136) H50(0.526185) H51(0.517816) H52(0.572177) H53(0.559075)
 H54(0.423878) H11(0.43364) H12(0.531353) H13A(0.602392) H13B(0.593425)
 H15A(0.510152) H15B(0.471877) H11A(0.510051) H11B(0.466961) H12A(0.576482)
 H12B(0.536912)
 Fixed Y: H1(-0.010028) H4A(0.173153) H4B(0.127007) H10(0.859238)
 H19(0.703653) H21(0.711777) H25(0.801317) H30(0.644599) H32(0.484653)
 H33(0.711138) H34(0.500933) H36(0.544208) H37(0.767636) H38(0.360049)
 H40(0.423353) H9A(0.210785) H9B(0.179896) H41(0.493437) H42(0.365052)
 H43(0.631994) H44(0.497769) H46(0.580123) H47(0.576793) H48(0.435825)
 H49(0.558237) H50(0.212381) H51(0.300186) H52(0.277281) H53(0.365875) H54(-
 0.104814) H11(-0.192668) H12(-0.038089) H13A(-0.115747) H13B(-0.057675) H15A(-
 0.263905) H15B(-0.261882) H11A(0.508712) H11B(0.474432) H12A(0.595968)
 H12B(0.563978)
 Fixed Z: O1(0.75) H1(0.616493) H4A(0.560739) H4B(0.547485) H10(0.904796)
 H19(0.95995) H21(0.895254) H25(1.006433) H30(0.861273) H32(1.020729)
 H33(0.984818) H34(0.854946) H36(0.923484) H37(0.883656) H38(0.872714)
 H40(0.912162) H9A(0.684887) H9B(0.71692) H41(0.995731) H42(0.814639)
 H43(0.965426) H44(0.876988) H46(0.78543) H47(0.760626) H48(0.811429)
 H49(0.899669) H50(0.856013) H51(0.881445) H52(0.76227) H53(0.786055)
 H54(0.674689) H11(0.705571) H12(0.788419) H13A(0.857006) H13B(0.841532)
 H15A(0.802048) H15B(0.764903) H11A(0.974721) H11B(0.954071) H12A(0.819703)
 H12B(0.799543)
;
_shelx_res_checksum              52138
_shelx_hkl_checksum              55583
_shelx_fab_checksum              68922
_platon_squeeze_void_probe_radius 1.20
_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 1.523
_oxdiff_exptl_absorpt_empirical_full_min 0.561