Unprecedented Water-Controlled Rotator–Stator Conversion of Supramolecular Rotor in Crystals
Huang, Rui-Kang; Xiao, Zhi-Feng; Liu, De-Xuan; Zhang, Wei-Xiong; Chen, Xiao-Ming; Chemical Communications  (2019) –; doi:10.1039/C9CC03267C

data_7123475
_publ_section_title
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 Unprecedented Water-Controlled Rotator--Stator Conversion of
 Supramolecular Rotor in Crystals
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03267C
_journal_year                    2019
_chemical_formula_moiety         'B F4, C12 H24 O6, C12 H12 N3'
_chemical_formula_sum            'C24 H36 B F4 N3 O6'
_chemical_formula_weight         549.37
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-22 deposited with the CCDC.    2019-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.5471(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.32950(13)
_cell_length_b                   18.8925(4)
_cell_length_c                   18.0731(3)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      76.1270
_cell_measurement_theta_min      2.4560
_cell_volume                     2819.44(9)
_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_temperature      260(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18299
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.997
_diffrn_reflns_theta_min         3.400
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32683
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         5245
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1148P)^2^+0.2396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.1801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4406
_reflns_number_total             5245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03267c2.cif
_cod_data_source_block           1ht
_cod_original_cell_volume        2819.44(8)
_cod_database_code               7123475
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C7A-C8A = C7B-C8B = C6B-C5B = C6A-C5A = C3B-C4B = C3A-C4A = C1B-C2B = C2A-C1A
 = C12B-C11B = C12A-C11A = C10B-C9B = C10A-C9A
 1.52 with sigma of 0.02
 O5A-C8A = O5B-C8B = O5A-C9A = O5B-C9B = O6A-C10A = O6B-C10B = O6A-C11A = O6B-
 C11B = O1A-C12A = O1B-C12B = O1A-C1A = O1B-C1B = O2A-C2A = O2B-C2B = O2B-C3B =
 O2A-C3A = O3A-C4A = O3B-C4B = O3B-C5B = O3A-C5A = O4A-C6A = O4B-C6B = O4A-C7A =
  O4B-C7B
 1.45 with sigma of 0.02
 N2B-C16B = N3B-C19B
 1.42 with sigma of 0.02
 F1B-F2B \\sim F1B-F3B \\sim F1B-F4B \\sim F2B-F3B \\sim F2B-F4B \\sim F3B-F4B
 with sigma of 0.04
 N3A-N2A \\sim N3B-N2B
 with sigma of 0.01
 F1A-F2A \\sim F1A-F3A \\sim F1A-F4A \\sim F2A-F3A \\sim F2A-F4A \\sim F3A-F4A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N2B \\sim N3B \\sim N2A \\sim N3A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B \\sim C11B \\sim C12B \\sim C1A \\sim C2A \\sim C3A \\sim C4A
\\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim
C12A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(C1B)=Sof(H1Ba)=
 Sof(H1Bb)=Sof(C2B)=Sof(H2Ba)=Sof(H2Bb)=Sof(C3B)=Sof(H3Ba)=Sof(H3Bb)=Sof(C4B)=
 Sof(H4Ba)=Sof(H4Bb)=Sof(C5B)=Sof(H5Ba)=Sof(H5Bb)=Sof(C6B)=Sof(H6Ba)=Sof(H6Bb)=
 Sof(C7B)=Sof(H7Ba)=Sof(H7Bb)=Sof(C8B)=Sof(H8Ba)=Sof(H8Bb)=Sof(C9B)=Sof(H9Ba)=
 Sof(H9Bb)=Sof(C10B)=Sof(H10c)=Sof(H10d)=Sof(C11B)=Sof(H11c)=Sof(H11d)=
 Sof(C12B)=Sof(H12c)=Sof(H12d)=Sof(N1B)=Sof(H1Bc)=Sof(H1Bd)=Sof(H1Be)=Sof(N2B)=
 Sof(N3B)=Sof(C16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18B)=Sof(C13B)=Sof(C14B)=
 Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(C24B)=Sof(H24B)=Sof(C19B)=Sof(C20B)=
 Sof(H20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(F1B)=
 Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(O2A)=Sof(N1A)=Sof(H1Ac)=Sof(H1Ad)=
 Sof(H1Ae)=Sof(O1A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(N2A)=Sof(N3A)=
 Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=Sof(C3A)=Sof(H3Aa)=
 Sof(H3Ab)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=Sof(C6A)=
 Sof(H6Aa)=Sof(H6Ab)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=
 Sof(C9A)=Sof(H9Aa)=Sof(H9Ab)=Sof(C10A)=Sof(H10a)=Sof(H10b)=Sof(C11A)=Sof(H11a)=
 Sof(H11b)=Sof(C12A)=Sof(H12a)=Sof(H12b)=Sof(C15A)=Sof(H15A)=Sof(C14A)=
 Sof(H14A)=Sof(C13A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17A)=Sof(C16A)=
 Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1B(H1Ba,H1Bb), C2B(H2Ba,H2Bb), C3B(H3Ba,H3Bb), C4B(H4Ba,H4Bb), C5B(H5Ba,
 H5Bb), C6B(H6Ba,H6Bb), C7B(H7Ba,H7Bb), C8B(H8Ba,H8Bb), C9B(H9Ba,H9Bb),
 C10B(H10c,H10d), C11B(H11c,H11d), C12B(H12c,H12d), C1A(H1Aa,H1Ab), C2A(H2Aa,
 H2Ab), C3A(H3Aa,H3Ab), C4A(H4Aa,H4Ab), C5A(H5Aa,H5Ab), C6A(H6Aa,H6Ab),
 C7A(H7Aa,H7Ab), C8A(H8Aa,H8Ab), C9A(H9Aa,H9Ab), C10A(H10a,H10b), C11A(H11a,
 H11b), C12A(H12a,H12b)
5.b Aromatic/amide H refined with riding coordinates:
 C17B(H17B), C18B(H18B), C14B(H14B), C15B(H15B), C24B(H24B), C20B(H20B),
 C21B(H21B), C22B(H22B), C23B(H23B), C15A(H15A), C14A(H14A), C18A(H18A),
 C17A(H17A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A)
5.c Fitted hexagon refined as free rotating group:
 C16B(C17B,C18B,C13B,C14B,C15B), C24B(C19B,C20B,C21B,C22B,C23B), C15A(C14A,
 C13A,C18A,C17A,C16A), C19A(C20A,C21A,C22A,C23A,C24A)
5.d Idealised Me refined as rotating group:
 N1A(H1Ac,H1Ad,H1Ae), N1B(H1Bc,H1Bd,H1Be)
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_olex2_submission_special_instructions 'No special instructions were received'