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_4514498
_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         'C111 H63 N26 O18 Zn8'
_chemical_formula_sum            'C111 H63 N26 O18 Zn8'
_chemical_formula_weight         2571.83
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                69.849(3)
_cell_angle_beta                 73.779(3)
_cell_angle_gamma                69.486(3)
_cell_formula_units_Z            2
_cell_length_a                   17.0241(5)
_cell_length_b                   18.1149(6)
_cell_length_c                   22.7218(8)
_cell_measurement_reflns_used    13012
_cell_measurement_temperature    99.99(14)
_cell_measurement_theta_max      66.5910
_cell_measurement_theta_min      3.7790
_cell_volume                     6060.0(4)
_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      99.99(14)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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    -29.00  60.00   0.50    5.00    --    0.00  68.00 -77.00  178
  2  \w    -42.00  -8.00   0.50    5.00    --    0.00 -68.00 149.00   68
  3  \w     91.00 122.00   0.50   10.00    --   83.30  68.00 -77.00   62
  4  \w     53.00  83.00   0.50   10.00    --   83.30 -68.00 149.00   60
  5  \w     -2.00  38.00   0.50    5.00    --    0.00  82.00-180.00   80
  6  \w    -38.00  22.00   0.50    5.00    --    0.00 -82.00 120.00  120
  7  \w    -27.00  -2.00   0.50    5.00    --    0.00  82.00 -60.00   50
  8  \w    -28.00  -3.00   0.50    5.00    --    0.00  82.00-180.00   50
  9  \w     -7.00  32.00   0.50    5.00    --    0.00 -82.00 -60.00   78
 10  \w    -38.00  32.00   0.50    5.00    --    0.00 -82.00-120.00  140
 11  \w     10.00  67.00   0.50   10.00    --   83.30 -77.00-120.00  114
 12  \w     52.00 153.00   0.50   10.00    --   83.30  19.00-180.00  202
 13  \w     -5.00  77.00   0.50   10.00    --   83.30 -82.00 -90.00  164
 14  \w     91.00 118.00   0.50   10.00    --   83.30 -82.00 -30.00   54
 15  \w     24.00 106.00   0.50   10.00    --   83.30 -38.00  60.00  164
 16  \w     32.00 118.00   0.50   10.00    --   83.30 -82.00  30.00  172
 17  \w      2.00  76.00   0.50   10.00    --   83.30 -82.00 -30.00  148
 18  \w     19.00  64.00   0.50   10.00    --   83.30 -77.00  60.00   90
 19  \w     -5.00 112.00   0.50   10.00    --   83.30 -82.00-150.00  234
 20  \w     58.00 168.00   0.50   10.00    --   83.30  57.00   0.00  220
 21  \w     91.00 116.00   0.50   10.00    --   83.30 -77.00-120.00   50
 22  \w     89.00 117.00   0.50   10.00    --   83.30 -82.00 -90.00   56
 23  \w     43.00 106.00   0.50   10.00    --   83.30 -38.00 -30.00  126
 24  \w     87.00 114.00   0.50   10.00    --   83.30 -82.00-180.00   54
 25  \w     80.00 114.00   0.50   10.00    --   83.30 -82.00  60.00   68
 26  \w     -6.00  42.00   0.50   10.00    --   83.30 -82.00  90.00   96
 27  \w     55.00  80.00   0.50   10.00    --   83.30 -82.00  90.00   50
 28  \w     86.00 111.00   0.50   10.00    --   83.30 -82.00  90.00   50
 29  \w     11.00  36.00   0.50   10.00    --   83.30 -38.00 -30.00   50
;
_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      0.0006137000
_diffrn_orient_matrix_UB_12      -0.0856387000
_diffrn_orient_matrix_UB_13      0.0458514000
_diffrn_orient_matrix_UB_21      0.0631608000
_diffrn_orient_matrix_UB_22      0.0062061000
_diffrn_orient_matrix_UB_23      0.0339810000
_diffrn_orient_matrix_UB_31      -0.0752320000
_diffrn_orient_matrix_UB_32      0.0392786000
_diffrn_orient_matrix_UB_33      0.0461998000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.1010
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64790
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.282
_diffrn_reflns_theta_max         67.282
_diffrn_reflns_theta_min         3.199
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    2.320
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60420
_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 dark pinkish '
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       needle
_exptl_crystal_F_000             2590
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.865
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1543
_refine_ls_number_reflns         20904
_refine_ls_number_restraints     413
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0780
_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^)+(0.1445P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2334
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11796
_reflns_number_total             20904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b14121_si_001.cif
_cod_data_source_block           1_beta
_cod_database_code               4514498
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O18-Zn8
 2 with sigma of 0.02
 C118-C112
 1.5 with sigma of 0.02
 O18-C112 = C112-O20
 1.22 with sigma of 0.02
 O17-C111 = C111-O19
 1.22 with sigma of 0.02
 C81-C106 \\sim C81-C115
 with sigma of 0.02
 C106-C107 \\sim C115-C114
 with sigma of 0.02
 C106-C105 \\sim C115-C116
 with sigma of 0.02
 C107-C108 \\sim C114-C113
 with sigma of 0.02
 C108-C109 \\sim C113-C118
 with sigma of 0.02
 C105-C110 \\sim C116-C117
 with sigma of 0.02
 C109-C110 \\sim C118-C117
 with sigma of 0.02
 C109-C111 \\sim C118-C111
 with sigma of 0.02
 C81-C107 \\sim C81-C114
 with sigma of 0.04
 C81-C105 \\sim C81-C116
 with sigma of 0.04
 C106-C108 \\sim C115-C113
 with sigma of 0.04
 C106-C110 \\sim C115-C117
 with sigma of 0.04
 C107-C105 \\sim C114-C116
 with sigma of 0.04
 C107-C109 \\sim C114-C118
 with sigma of 0.04
 C107-C112 \\sim C114-C112
 with sigma of 0.04
 C108-C110 \\sim C113-C117
 with sigma of 0.04
 C108-C111 \\sim C113-C111
 with sigma of 0.04
 C108-C112 \\sim C113-C112
 with sigma of 0.04
 C105-C109 \\sim C116-C118
 with sigma of 0.04
 C109-C112 \\sim C118-C112
 with sigma of 0.04
 C110-C111 \\sim C117-C111
 with sigma of 0.04
 C110-C112 \\sim C117-C112
 with sigma of 0.04
 C113-C112 \\sim C112-C117
 with sigma of 0.02
 O18-C118 \\sim C118-O20
 with sigma of 0.02
 O17-C109 \\sim C109-O19
 with sigma of 0.02
 C110-C111 \\sim C111-C108
 with sigma of 0.02
3. Restrained planarity
 C118, C113, C117, C112
 with sigma of 0.005
 C109, C111, O17, O19
 with sigma of 0.005
 C110, C109, C108, C111
 with sigma of 0.005
 O17, C111, O19, C109
 with sigma of 0.005
4. Rigid bond restraints
 O17, C105, C106, C107, C108, C109, C110, O19, C111
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 O18, O20, C112, C113, C114, C115, C116, C117, C118
 with sigma for 1-2 distances of 0.0105 and sigma for 1-3 distances of 0.01
 O15, C104, O16, C103, C101, C97, C75, C100, C102
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O17 \\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim O19
\\sim C111: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
O18 \\sim O20 \\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117
\\sim C118: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C75 \\sim C100 \\sim C102 \\sim C103 \\sim C101 \\sim C97 \\sim O15 \\sim C104
\\sim O16: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O17) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C107)
\\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(O19) \\sim Ueq, Uanis(C111) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(O18) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C113)
\\sim Ueq, Uanis(C114) \\sim Ueq, Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq,
Uanis(C117) \\sim Ueq, Uanis(C118) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C75) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(C103)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(O16) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
6. Others
 Fixed Sof: O17(0.5) O18(0.5) C105(0.5) C106(0.5) C107(0.5) C108(0.5)
 C109(0.5) C110(0.5) O19(0.5) O20(0.5) C111(0.5) C112(0.5) C113(0.5) H113(0.5)
 C114(0.5) H114(0.5) C115(0.5) C116(0.5) H116(0.5) C117(0.5) H117(0.5) C118(0.5)
7.a Rotating group:
 N15(H15A,H15B), O12(H12A,H12B), N21(H21A,H21B), N22(H22A,H22B), N23(H23A,
 H23B), N26(H26A,H26B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C25(H25), C27(H27), C29(H29), C30(H30), C33(H33), C38(H38),
 C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C47(H47), C48(H48), C51(H51),
  C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C60(H60), C61(H61),
 C62(H62), C63(H63), C64(H64), C66(H66), C69(H69), C76(H76), C77(H77), C79(H79),
  C84(H84), C85(H85), C86(H86), C89(H89), C90(H90), C91(H91), C93(H93),
 C94(H94), C95(H95), C96(H96), C97(H97), C98(H98), C99(H99), C100(H100),
 C101(H101), C102(H102), C113(H113), C114(H114), C116(H116), C117(H117)
7.c Fitted hexagon refined as free rotating group:
 C105(C106,C107,C108,C109,C110)
7.d X=CH2 refined with riding coordinates:
 N25(H25A,H25B)
;
_shelx_res_checksum              10779
_shelx_hkl_checksum              66741
_shelx_fab_checksum              6241
_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 2.895
_oxdiff_exptl_absorpt_empirical_full_min 0.738