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_4514499
_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 H61 N26 O21 Zn8'
_chemical_formula_sum            'C111 H61 N26 O21 Zn8'
_chemical_formula_weight         2617.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-06-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.383(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5074(9)
_cell_length_b                   29.3383(12)
_cell_length_c                   26.3661(14)
_cell_measurement_reflns_used    8158
_cell_measurement_temperature    99.99(14)
_cell_measurement_theta_max      59.4960
_cell_measurement_theta_min      2.8350
_cell_volume                     15219.1(13)
_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)'
_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    -45.00  22.00   0.50    9.31    --    0.00 -53.00 -16.00  134
  2  \w    -85.00 -50.00   0.50    9.31    --    0.00 -53.00 -16.00   70
  3  \w     -7.00  42.00   0.50   37.00    --   79.40 -53.00 -16.00   98
  4  \w     88.00 113.00   0.50   37.00    --   79.40  53.00 127.00   50
  5  \w      8.00  33.00   0.50    9.31    --    0.00  53.00 127.00   50
  6  \w     77.00 169.00   0.50   37.00    --   79.40  77.00  60.00  184
  7  \w     57.00  82.00   0.50   37.00    --   79.40  38.00 -90.00   50
  8  \w     82.00 114.00   0.50   37.00    --   79.40  82.00  90.00   64
  9  \w    120.00 168.00   0.50   37.00    --   79.40  82.00  90.00   96
 10  \w     76.00 160.00   0.50   37.00    --   79.40  77.00-150.00  168
 11  \w     82.00 169.00   0.50   37.00    --   79.40  82.00-180.00  174
 12  \w     86.00 130.00   0.50   37.00    --   79.40  38.00 -90.00   88
 13  \w    144.00 169.00   0.50   37.00    --   79.40  38.00 -90.00   50
 14  \w     82.00 167.00   0.50   37.00    --   79.40  82.00 -30.00  170
 15  \w      8.00  33.00   0.50    9.31    --    0.00  53.00 127.00   50
 16  \w    -29.00   0.00   0.50    9.31    --    0.00 -82.00-120.00   58
 17  \w      8.00  39.00   0.50    9.31    --    0.00  82.00 -30.00   62
 18  \w    -25.00   0.00   0.50    9.31    --    0.00  82.00 -30.00   50
 19  \w    -27.00   0.00   0.50    9.31    --    0.00  82.00-150.00   54
 20  \w    -36.00 -11.00   0.50    9.31    --    0.00 -82.00  30.00   50
 21  \w      8.00  34.00   0.50    9.31    --    0.00 -82.00  30.00   52
 22  \w    -14.00  29.00   0.50    9.31    --    0.00 -82.00 -60.00   86
 23  \w     84.00 135.00   0.50   37.00    --   79.40  82.00  30.00  102
 24  \w     62.00  93.00   0.50   37.00    --   79.40 -38.00-180.00   62
 25  \w     -1.00  25.00   0.50   37.00    --   79.40 -38.00-180.00   52
 26  \w     76.00 102.00   0.50   37.00    --   79.40  77.00   0.00   52
 27  \w     34.00  76.00   0.50   37.00    --   79.40 -38.00  90.00   84
 28  \w     -8.00  21.00   0.50   37.00    --   79.40 -38.00  90.00   58
;
_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      0.0306747000
_diffrn_orient_matrix_UB_12      -0.0192712000
_diffrn_orient_matrix_UB_13      0.0561094000
_diffrn_orient_matrix_UB_21      0.0514586000
_diffrn_orient_matrix_UB_22      -0.0279334000
_diffrn_orient_matrix_UB_23      -0.0199109000
_diffrn_orient_matrix_UB_31      0.0504194000
_diffrn_orient_matrix_UB_32      0.0400573000
_diffrn_orient_matrix_UB_33      0.0129600000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1293
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            116531
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        65.376
_diffrn_reflns_theta_max         65.376
_diffrn_reflns_theta_min         2.704
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67890
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       needle
_exptl_crystal_F_000             5268
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.891
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1440
_refine_ls_number_reflns         25137
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.2302
_refine_ls_R_factor_gt           0.1432
_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^)+(0.2200P)^2^+12.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3601
_refine_ls_wR_factor_ref         0.4287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10265
_reflns_number_total             25137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b14121_si_001.cif
_cod_data_source_block           1_gamma
_cod_original_cell_volume        15219.2(13)
_cod_database_code               4514499
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.946
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     59.94
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 C94-C110
 1.52 with sigma of 0.02
 O15-C110 = C110-O17
 1.22 with sigma of 0.02
 C103-C112
 1.53 with sigma of 0.02
 O19-C112 = C112-O18
 1.23 with sigma of 0.02
 O19-O18
 2.222 with sigma of 0.02
 O6-C23 = C23-O7
 1.23 with sigma of 0.02
 O6-O7
 2.22 with sigma of 0.02
 C93-C110 \\sim C110-C95
 with sigma of 0.02
 O17-C94 \\sim C94-O15
 with sigma of 0.02
 C102-C112 \\sim C112-C104
 with sigma of 0.02
 O19-C103 \\sim C103-O18
 with sigma of 0.02
 C104-C112 \\sim C112-C102
 with sigma of 0.02
 C11-C23 \\sim C23-C9
 with sigma of 0.02
 O6-C10 \\sim C10-O7
 with sigma of 0.02
3. Restrained planarity
 O15, O17, C110, C94
 with sigma of 0.005
 C93, C94, C95, C110
 with sigma of 0.005
 C103, O18, O19, C112
 with sigma of 0.005
 C102, C103, C104, C112
 with sigma of 0.005
 O6, O7, C23, C10
 with sigma of 0.005
4. Rigid bond restraints
 C102, C103, C104, C105, C106, C107, O18, O19, C112
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 O15, O17, C91, C92, C93, C94, C95, C96, C110
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 N18, N21, C38, C39, N22, C40, N23, N24, C109, N26, C111
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim O18 \\sim O19
\\sim C112: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
O15 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C110
\\sim O17: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
N18 \\sim N21 \\sim C38 \\sim C39 \\sim N22 \\sim C40 \\sim N23 \\sim N24 \\sim
C109 \\sim N26 \\sim C111: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(O18)
\\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(C112) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
Uanis(O15) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C96) \\sim Ueq,
Uanis(C110) \\sim Ueq, Uanis(C91) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(N18) \\sim Ueq, Uanis(N21) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(N22) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(N23) \\sim Ueq,
Uanis(N24) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(N26) \\sim Ueq, Uanis(C111)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C48) = Uanis(C27)
Uanis(C44) = Uanis(C70)
6.a Rotating group:
 N7(H7A,H7B), N12(H12A,H12B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C9(H9), C11(H11), C12(H12), C16(H16), C21(H21),
 C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C40(H40),
  C44(H44), C45(H45), C47(H47), C53(H53), C54(H54), C56(H56), C59(H59),
 C62(H62), C65(H65), C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C77(H77),
  C78(H78), C80(H80), C84(H84), C85(H85), C89(H89), C92(H92), C93(H93),
 C95(H95), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102),
 C104(H104), C105(H105), C107(H107), C108(H108)
6.c Fitted pentagon refined as free rotating group:
 N21(C38,C39,N22,C40)
6.d Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C11,C12), C91(C92,C93,C94,C95,C96), C102(C103,C104,C105,C106,C107)
6.e X=CH2 refined with riding coordinates:
 N20(H20A,H20B), N24(H24A,H24B), N25(H25A,H25B), N26(H26A,H26B)
;
_shelx_res_checksum              20008
_shelx_hkl_checksum              38433
_shelx_fab_checksum              75558
_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 1.484
_oxdiff_exptl_absorpt_empirical_full_min 0.663