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_7123476
_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         'C12 H24 O6, C12 H12 N3, B F4'
_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                 96.2603(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.25835(10)
_cell_length_b                   18.7293(2)
_cell_length_c                   17.91116(19)
_cell_measurement_reflns_used    13327
_cell_measurement_temperature    170
_cell_measurement_theta_max      77.1850
_cell_measurement_theta_min      2.3430
_cell_volume                     2753.85(5)
_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      170.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18872
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_min         3.425
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62623
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.325
_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         0.280
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.00086(11)
_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   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5130
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0421P)^2^+0.6095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4823
_reflns_number_total             5130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03267c2.cif
_cod_data_source_block           1lt
_cod_original_cell_volume        2753.85(6)
_cod_database_code               7123476
_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
 N2B-C16B \\sim N2A-C16A \\sim N3A-C19A \\sim N3B-C19B
 with sigma of 0.01
 N3A-N2A \\sim N3B-N2B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N3B \\sim N3A \\sim N2B \\sim N2A: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008
Uanis(C13B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(F1B)=Sof(F4B)=Sof(F3B)=Sof(F2B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F4A)=Sof(F3A)=FVAR(1)
 Sof(N3B)=Sof(N1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C18B)=Sof(H18B)=Sof(C13B)=
 Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(C17B)=Sof(H17B)=Sof(N2B)=
 Sof(C24B)=Sof(H24B)=Sof(C19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=1-FVAR(2)
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C16A)=Sof(C15A)=Sof(H15A)=
 Sof(C14A)=Sof(H14A)=Sof(C13A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17A)=Sof(N2A)=
 Sof(N3A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C6(H6A,H6B), C11(H11A,H11B), C5(H5A,H5B), C1(H1A,H1B), C2(H2A,
 H2B), C4(H4A,H4B), C8(H8A,H8B), C3(H3A,H3B), C10(H10A,H10B), C7(H7A,H7B),
 C9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C15A(H15A), C14A(H14A), C18A(H18A), C17A(H17A), C20A(H20A), C21A(H21A),
 C22A(H22A), C23A(H23A), C24A(H24A), C18B(H18B), C14B(H14B), C15B(H15B),
 C17B(H17B), C24B(H24B), C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B)
5.c Fitted hexagon refined as free rotating group:
 C16A(C15A,C14A,C13A,C18A,C17A), C19A(C20A,C21A,C22A,C23A,C24A), C18B(C13B,
 C14B,C15B,C16B,C17B), C24B(C19B,C20B,C21B,C22B,C23B)
5.d Idealised Me refined as rotating group:
 N1A(H1AA,H1AB,H1AC), N1B(H1BA,H1BB,H1BC)
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_shelx_res_checksum              272
_olex2_submission_special_instructions 'No special instructions were received'