Visible-Light-Driven Rotation of Molecular Motors in Discrete Supramolecular Metallacycles
Shi, Zhao-Tao; Hu, Yi-Xiong; Hu, Zhubin; Zhang, Qi; Chen, Shao-Yu; Chen, Meng; Yu, Jing-Jing; Yin, Guang-Qiang; Sun, Haitao; Xu, Lin; Li, Xiaopeng; Feringa, Ben L.; Yang, Hai-Bo; Tian, He; Qu, Da-Hui; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11752

data_4135429
_publ_section_title
;
 Visible-Light-Driven Rotation of Molecular Motors in Discrete
 Supramolecular Metallacycles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11752
_journal_year                    2020
_chemical_formula_moiety         'C37 H26 N2 O2'
_chemical_formula_sum            'C37 H26 N2 O2'
_chemical_formula_weight         530.63
_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_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-28
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_cell_angle_alpha                83.8430(10)
_cell_angle_beta                 88.7230(10)
_cell_angle_gamma                69.5970(10)
_cell_formula_units_Z            4
_cell_length_a                   10.9265(5)
_cell_length_b                   12.9671(6)
_cell_length_c                   21.9636(10)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    293
_cell_measurement_theta_max      47.566
_cell_measurement_theta_min      4.366
_cell_volume                     2899.5(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.31
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57852
_diffrn_reflns_theta_full        27.5298
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6761
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.2155
_exptl_crystal_description       block
_exptl_crystal_F_000             1112.4867
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.3351
_refine_diff_density_min         -0.3383
_refine_diff_density_rms         0.0738
_refine_ls_d_res_high            0.7688
_refine_ls_d_res_low             10.9170
_refine_ls_goodness_of_fit_ref   1.0680
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    98
_refine_ls_number_parameters     741
_refine_ls_number_reflns         13320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0680
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.2059
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                7255
_reflns_number_total             13320
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c11752_si_002.cif
_cod_data_source_block           mo_d8v19261_0m
_cod_database_code               4135429
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Ternary CH refined with riding coordinates: 
 C25(H25), C62(H62) 
2.b Secondary CH2 refined with riding coordinates: 
 C26(H26a,H26b), C63(H63a,H63b) 
2.c Aromatic/amide H refined with riding coordinates: 
 C2(H2), C4(H4), C5(H5), C12(H12), C10(H10), C9(H9), C29(H29), C28(H28), 
 C34(H34), C33(H33), C32(H32), C31(H31), C39(H39), C41(H41), C42(H42), C46(H46), 
  C47(H47), C49(H49), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), 
 C71(H71), C22(H22), C21(H21), C20(H20), C23(H23), C16(H16), C17(H17), C18(H18), 
  C15(H15), C58(H58), C59(H59), C60(H60), C57(H57), C53(H53), C54(H54), 
 C55(H55), C52(H52) 
2.d Idealised Me refined as rotating group: 
 C37(H37a,H37b,H37c), C74(H74a,H74b,H74c) 
;
_olex2_submission_special_instructions 'No special instructions were received'