Dynamic Topochemical Reaction Tuned by Guest Molecules in the Nanospace of a Metal-Organic Framework.
Kusaka, Shinpei; Kiyose, Atsushi; Sato, Hiroshi; Hijikata, Yuh; Hori, Akihiro; Ma, Yunsheng; Matsuda, Ryotaro; Journal of the American Chemical Society 141 (2019) 15742–15746; doi:10.1021/jacs.9b07682

data_4128318
_publ_section_title
;
 Dynamic Topochemical Reaction Tuned by Guest Molecules in the Nanospace
 of a Metal-Organic Framework.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15742
_journal_page_last               15746
_journal_paper_doi               10.1021/jacs.9b07682
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C27 H19 N O4 Zn'
_chemical_formula_sum            'C27.41 H19.41 N O4 Zn'
_chemical_formula_weight         492.14
_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   geom
_audit_creation_date             2018-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                88.301(5)
_cell_angle_beta                 86.590(5)
_cell_angle_gamma                80.201(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8030(6)
_cell_length_b                   9.8836(6)
_cell_length_c                   11.8009(8)
_cell_measurement_reflns_used    5976
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.09
_cell_volume                     1124.48(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9b (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    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93.15
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20299
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.327
_diffrn_reflns_theta_min         2.092
_exptl_absorpt_coefficient_mu    1.127
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            nONE
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       nONE
_exptl_crystal_F_000             506
_refine_diff_density_max         1.789
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5915
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0784
_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^)+(0.1365P)^2^+1.4910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4206
_reflns_number_total             5915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07682_si_003.cif
_cod_data_source_block           xcalibur
_cod_database_code               4128318
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C40-C41
 1.58 with sigma of 0.01
 C41-C40_$1
 1.58 with sigma of 0.01
 C39-C40 = C41-C42
 1.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C52 \\sim C55 \\sim C51 \\sim C56 \\sim C50 \\sim C53 \\sim C57 \\sim C58 \\sim
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim N35: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C39 \\sim C41 \\sim C40 \\sim C36 \\sim C35 \\sim N34 \\sim C42 \\sim C43 \\sim
C44 \\sim C45 \\sim C46 \\sim C47 \\sim C38 \\sim C37: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 N34, C35, C36, C39, C38, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C55)=Sof(H55)=Sof(C51)=Sof(H51)=Sof(C50)=Sof(H50)=Sof(N35)=Sof(C63)=
 Sof(H63)=Sof(C53)=Sof(H53)=Sof(C52)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(C58)=
 Sof(H58)=Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=Sof(C62)=
 Sof(H62)=1-FVAR(1)
 Sof(C39)=Sof(C36)=Sof(H36)=Sof(C35)=Sof(H35)=Sof(N34)=Sof(C37)=Sof(H37)=
 Sof(C38)=Sof(H38)=Sof(C41)=Sof(H41)=Sof(C40)=Sof(H40)=Sof(C42)=Sof(C43)=
 Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=
 Sof(H47)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C41(H41), C40(H40)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C16(H16), C11(H11), C8(H8), C12(H12), C15(H15), C9(H9),
 C36(H36), C35(H35), C37(H37), C38(H38), C43(H43), C44(H44), C45(H45), C46(H46),
  C47(H47), C55(H55), C51(H51), C50(H50), C63(H63), C53(H53), C56(H56),
 C58(H58), C59(H59), C60(H60), C61(H61), C62(H62)
6.c Fitted hexagon refined as free rotating group:
 C39(C36,C35,N34,C37,C38), C42(C43,C44,C45,C46,C47), C51(C50,N35,C63,C53,C52),
 C57(C58,C59,C60,C61,C62)
;
_shelx_res_checksum              98066
_shelx_hkl_checksum              33589
_olex2_submission_special_instructions 'No special instructions were received'