Multi-Stimuli Responsive Interconversion between Bowl- and Capsule-Shaped Self-Assembled Zinc(II) Complexes.
Endo, Kenichi; Ube, Hitoshi; Shionoya, Mitsuhiko; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b11099

data_4133802
_publ_section_title
;
 Multi-Stimuli Responsive Interconversion between Bowl- and Capsule-Shaped
 Self-Assembled Zinc(II) Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11099
_journal_year                    2019
_chemical_formula_moiety
'C224 H144 N44 O4 Zn8, 10(C F3 O3 S), C6 H14 O, 8(C2 H3 N), 2(O)'
_chemical_formula_sum            'C256 H182 F30 N52 O37 S10 Zn8'
_chemical_formula_weight         5992.09
_chemical_properties_physical    Efflorescent
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.0230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4244(3)
_cell_length_b                   38.6332(6)
_cell_length_c                   35.0018(7)
_cell_measurement_reflns_used    44042
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      73.1120
_cell_measurement_theta_min      2.5290
_cell_volume                     31655.5(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.968
_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    -37.00 -10.00   0.50    0.86    --    0.00 -38.00-180.00   54
  2  \w    -85.00 -39.00   0.50    0.86    --    0.00 -38.00-180.00   92
  3  \w    -86.00   7.00   0.50    0.86    --    0.00 -57.00 -30.00  186
  4  \w    -58.00  24.00   0.50    0.86    --    0.00 -38.00   0.00  164
  5  \w     73.00 177.00   0.50    3.43    --   98.20  45.00 -60.00  208
  6  \w     10.00 132.00   0.50    3.43    --   98.20 -82.00  60.00  244
  7  \w    150.00 179.00   0.50    3.43    --   98.20  30.00-120.00   58
  8  \w     99.00 151.00   0.50    3.43    --   98.20  30.00-180.00  104
  9  \w     10.00 120.00   0.50    3.43    --   98.20 -82.00  30.00  220
 10  \w     84.00 109.00   0.50    3.43    --   98.20  45.00  30.00   50
 11  \w     21.00  54.00   0.50    3.43    --   98.20 -45.00  90.00   66
 12  \w     94.00 120.00   0.50    3.43    --   98.20 -45.00  90.00   52
 13  \w     67.00 137.00   0.50    3.43    --   98.20  30.00-120.00  140
 14  \w     11.00 120.00   0.50    3.43    --   98.20 -61.00  60.00  218
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0638685000
_diffrn_orient_matrix_UB_12      -0.0095828000
_diffrn_orient_matrix_UB_13      -0.0006053000
_diffrn_orient_matrix_UB_21      -0.0159039000
_diffrn_orient_matrix_UB_22      0.0382296000
_diffrn_orient_matrix_UB_23      -0.0069838000
_diffrn_orient_matrix_UB_31      0.0010959000
_diffrn_orient_matrix_UB_32      -0.0060929000
_diffrn_orient_matrix_UB_33      -0.0434621000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            178784
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        68.250
_diffrn_reflns_theta_max         73.673
_diffrn_reflns_theta_min         2.287
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       plate
_exptl_crystal_F_000             12192
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/diisopropyl ether'
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.940
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3723
_refine_ls_number_reflns         61915
_refine_ls_number_restraints     745
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0921
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1203P)^2^+180.0820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2506
_refine_ls_wR_factor_ref         0.2709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                44163
_reflns_number_total             61915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11099_si_003.cif
_cod_data_source_block           Zn4L4
_cod_database_code               4133802
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHNOSFZn
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.339
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H44D,H44E,H44F} of C441, All C(H,H) groups
 At 1.5 times of:
  {H41A,H41B,H41C} of C416, {H44A,H44B,H44C} of C446, {H40A,H40B,H40C} of
  C409, {H15A,H15B,H15C} of C153, {H31D,H31E,H31F} of C314, {H38A,H38B,H38C} of
  C387, {H20A,H20B,H20C} of C202, {H31G,H31H,H31I} of C315, {H34A,H34B,H34C} of
  C344, {H31A,H31B,H31C} of C313, {H26A,H26B,H26C} of C269, {H30A,H30B,H30C} of
  C309, {H39D,H39E,H39F} of C398, {H39A,H39B,H39C} of C393, {H39G,H39H,H39I} of
  C390
2. Uiso/Uaniso restraints and constraints
S80 \\sim F91 \\sim F92 \\sim F93 \\sim O325 \\sim O326 \\sim O327 \\sim C3
\\sim S80A \\sim F91A \\sim F92A \\sim F93A \\sim O1 \\sim O2 \\sim O3 \\sim
C3A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
S1 \\sim F5 \\sim F22 \\sim F26 \\sim O23 \\sim O334 \\sim O335 \\sim C467
\\sim S77 \\sim F82 \\sim F83 \\sim F84 \\sim O85 \\sim O312 \\sim O313 \\sim
C83: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C2 \\sim C292 \\sim C293 \\sim C1 \\sim C4 \\sim C294: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 S80A, F91A, F92A, F93A, O1, O2, O3, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S77, F82, F83, F84, O85, O312, O313, C83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1, F5, F22, F26, O23, O334, O335, C467
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{S77, F82, F83, F84, O85, O312, O313, C83} sigma for 1-2: 0.02, 1-3: 0.04
as
{S1, F5, F22, F26, O23, O334, O335, C467}
{S11, F9, F15, F16, O12, O13, O14, C10} sigma for 1-2: 0.02, 1-3: 0.04
as
{S80, F91, F92, F93, O325, O326, O327, C3}
{S11, F9, F15, F16, O12, O13, O14, C10} sigma for 1-2: 0.02, 1-3: 0.04
as
{S80A, F91A, F92A, F93A, O1, O2, O3, C3A}
5. Others
 Sof(H29A)=Sof(S80A)=Sof(F91A)=Sof(F92A)=Sof(F93A)=Sof(O1)=Sof(O2)=Sof(O3)=
 Sof(C3A)=Sof(C2)=Sof(H2)=Sof(C1)=Sof(H1)=Sof(C4)=Sof(H4)=1-FVAR(1)
 Sof(C292)=Sof(H292)=Sof(C293)=Sof(H293)=Sof(C294)=Sof(H294)=Sof(H295)=
 Sof(S80)=Sof(F91)=Sof(F92)=Sof(F93)=Sof(O325)=Sof(O326)=Sof(O327)=Sof(C3)=
 FVAR(1)
 Sof(S1)=Sof(F5)=Sof(F22)=Sof(F26)=Sof(O23)=Sof(O334)=Sof(O335)=Sof(C467)=1-
 FVAR(2)
 Sof(S77)=Sof(F82)=Sof(F83)=Sof(F84)=Sof(O85)=Sof(O312)=Sof(O313)=Sof(C83)=
 FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C310(H310), C312(H312)
6.b Me refined with riding coordinates:
 C309(H30A,H30B,H30C), C313(H31A,H31B,H31C), C314(H31D,H31E,H31F), C315(H31G,
 H31H,H31I)
6.c Aromatic/amide H refined with riding coordinates:
 C115(H115), C116(H116), C117(H117), C118(H118), C119(H119), C120(H120),
 C122(H122), C124(H124), C125(H125), C128(H128), C129(H129), C130(H130),
 C131(H131), C134(H134), C135(H135), C137(H137), C140(H140), C141(H141),
 C143(H143), C145(H145), C146(H146), C148(H148), C149(H149), C151(H151),
 C152(H152), C155(H155), C156(H156), C159(H159), C162(H162), C163(H163),
 C164(H164), C165(H165), C190(H190), C191(H191), C192(H192), C193(H193),
 C194(H194), C195(H195), C196(H196), C197(H197), C199(H199), C200(H200),
 C204(H204), C205(H205), C207(H207), C210(H210), C211(H211), C212(H212),
 C213(H213), C215(H215), C216(H216), C218(H218), C220(H220), C221(H221),
 C225(H225), C226(H226), C227(H227), C228(H228), C230(H230), C232(H232),
 C233(H233), C237(H237), C238(H238), C239(H239), C240(H240), C257(H257),
 C258(H258), C259(H259), C260(H260), C261(H261), C262(H262), C263(H263),
 C264(H264), C266(H266), C267(H267), C271(H271), C272(H272), C274(H274),
 C277(H277), C278(H278), C279(H279), C280(H280), C282(H282), C283(H283),
 C285(H285), C287(H287), C288(H288), C292(H292), C293(H293), C294(H294),
 C295(H295), C295(H29A), C297(H297), C299(H299), C300(H300), C304(H304),
 C305(H305), C306(H306), C307(H307), C332(H332), C333(H333), C334(H334),
 C335(H335), C336(H336), C337(H337), C338(H338), C339(H339), C341(H341),
 C342(H342), C347(H347), C348(H348), C350(H350), C352(H352), C353(H353),
 C354(H354), C355(H355), C357(H357), C358(H358), C360(H360), C362(H362),
 C363(H363), C367(H367), C368(H368), C369(H369), C370(H370), C372(H372),
 C374(H374), C375(H375), C379(H379), C380(H380), C381(H381), C382(H382),
 C445(H445), C2(H2), C1(H1), C4(H4)
6.d Idealised Me refined as rotating group:
 C153(H15A,H15B,H15C), C202(H20A,H20B,H20C), C269(H26A,H26B,H26C), C344(H34A,
 H34B,H34C), C393(H39A,H39B,H39C), C387(H38A,H38B,H38C), C398(H39D,H39E,H39F),
 C409(H40A,H40B,H40C), C390(H39G,H39H,H39I), C446(H44A,H44B,H44C), C416(H41A,
 H41B,H41C), C441(H44D,H44E,H44F)
;
_shelx_res_checksum              4716
_shelx_hkl_checksum              67704
_shelx_fab_checksum              64967
_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 2.075
_oxdiff_exptl_absorpt_empirical_full_min 0.522