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_7123477
_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         '0.5(H2 O), B F4, C12 H24 O6, C12 H12 N3'
_chemical_formula_sum            'C24 H37 B F4 N3 O6.5'
_chemical_formula_weight         558.37
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-20
_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                 101.962(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5409(2)
_cell_length_b                   19.0473(4)
_cell_length_c                   18.1701(3)
_cell_measurement_reflns_used    40510
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      77.3850
_cell_measurement_theta_min      2.2990
_cell_volume                     2891.74(10)
_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 0.986
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19216
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.982
_diffrn_reflns_theta_min         3.401
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         5382
_refine_ls_number_restraints     309
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0565
_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^)+(0.1071P)^2^+0.2287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4350
_reflns_number_total             5382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03267c2.cif
_cod_data_source_block           1wht
_cod_original_formula_sum        'C24 H37 B F4 N3 O6.50'
_cod_database_code               7123477
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.654
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N2A-N3A = N2B-N3B
 1.25 with sigma of 0.01
 C10B-C11B = N2A-C19A = N3B-C16B
 2.4 with sigma of 0.04
 N2A-C16A = N3A-C19A = N2B-C16B = N3B-C19B
 1.42 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2A \\sim N3A \\sim N2B \\sim N3B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A \\sim C10A \\sim C11A \\sim C12A \\sim C1B \\sim C2B \\sim C3B \\sim C4B
\\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim C9B \\sim C10B \\sim C11B \\sim
C12B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim O6A \\sim O1B \\sim O2B \\sim
O3B \\sim O4B \\sim O5B \\sim O6B: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=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(C13B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=
 Sof(H15B)=Sof(C16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18B)=Sof(C21B)=
 Sof(H21B)=Sof(C20B)=Sof(H20B)=Sof(C19B)=Sof(C24B)=Sof(H24B)=Sof(C23B)=
 Sof(H23B)=Sof(C22B)=Sof(H22B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=
 Sof(O5A)=Sof(O6A)=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(N1A)=Sof(H1AC)=
 Sof(H1AD)=Sof(H1AE)=Sof(N2A)=Sof(N3A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=
 Sof(H15A)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(C24A)=Sof(H24A)=Sof(C23A)=Sof(H23A)=Sof(C22A)=Sof(H22A)=Sof(C21A)=
 Sof(H21A)=Sof(C20A)=Sof(H20A)=FVAR(1)
 Fixed Sof: O7(0.5) H7A(0.5) H7B(0.5)
5.a Free rotating group:
 O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 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), 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)
5.c Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C15A(H15A), C17A(H17A), C18A(H18A), C24A(H24A), C23A(H23A),
 C22A(H22A), C21A(H21A), C20A(H20A), C14B(H14B), C15B(H15B), C17B(H17B),
 C18B(H18B), C21B(H21B), C20B(H20B), C24B(H24B), C23B(H23B), C22B(H22B)
5.d Fitted hexagon refined as free rotating group:
 C19A(C24A,C23A,C22A,C21A,C20A), C13B(C14B,C15B,C16B,C17B,C18B), C21B(C20B,
 C19B,C24B,C23B,C22B)
5.e Idealised Me refined as rotating group:
 N1A(H1AC,H1AD,H1AE), N1B(H1BC,H1BD,H1BE)
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_shelx_res_checksum              95226
_olex2_submission_special_instructions 'No special instructions were received'