Molecular Turnstiles Regulated by Metal Ions.
Wang, Guangxia; Xiao, Hongmei; He, Jiaojiao; Xiang, Junfeng; Wang, Ying; Chen, Xuebo; Che, Yanke; Jiang, Hua; The Journal of organic chemistry 81 (2016) 3364–3371; doi:10.1021/acs.joc.6b00463

data_4036767
_publ_section_title
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 Molecular Turnstiles Regulated by Metal Ions.
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_journal_issue                   8
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3364
_journal_page_last               3371
_journal_paper_doi               10.1021/acs.joc.6b00463
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C56 H36 N2 O4'
_chemical_formula_sum            'C56 H36 N2 O4'
_chemical_formula_weight         800.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                89.312(5)
_cell_angle_beta                 75.124(5)
_cell_angle_gamma                87.829(6)
_cell_formula_units_Z            2
_cell_length_a                   9.1134(11)
_cell_length_b                   13.830(2)
_cell_length_c                   16.661(2)
_cell_measurement_reflns_used    7211
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4761
_cell_measurement_theta_min      1.2646
_cell_volume                     2028.1(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution
;
'SHELXS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.1114
_diffrn_orient_matrix_UB_12      0.0138
_diffrn_orient_matrix_UB_13      -0.0175
_diffrn_orient_matrix_UB_21      -0.0151
_diffrn_orient_matrix_UB_22      0.0647
_diffrn_orient_matrix_UB_23      -0.0285
_diffrn_orient_matrix_UB_31      -0.0101
_diffrn_orient_matrix_UB_32      0.0226
_diffrn_orient_matrix_UB_33      0.0570
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24590
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.940
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         9243
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0570P)^2^+0.5676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8526
_reflns_number_total             9243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00463_si_002.cif
_cod_data_source_block           mx3267
_cod_original_cell_volume        2028.2(5)
_cod_database_code               4036767
_shelxl_version_number           2013-4
_diffrn_number_total             9245
_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. Uiso/Uaniso restraints and constraints
C52A \\sim C52 \\sim N2A \\sim N2: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.08
Uanis(N2) \\sim Ueq, Uanis(C52A) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(N2A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H50A)=Sof(H51A)=Sof(H53A)=Sof(C52A)=Sof(H52A)=Sof(N2A)=1-FVAR(1)
 Sof(N2)=Sof(H50)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(H53)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C55(H55A,H55B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21),
 C22(H22), C23(H23), C24(H24), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
  C35(H35), C36(H36), C37(H37), C42(H42), C43(H43), C45(H45), C50(H50),
 C50(H50A), C51(H51), C51(H51A), C52(H52), C53(H53), C53(H53A), C52A(H52A)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C56(H56A,H56B,H56C)
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_shelx_res_checksum              39699
_shelx_hkl_checksum              27654