Flexible, Linear Chains Act as Baffles To Inhibit the Intramolecular Rotation of Molecular Turnstiles.
Yu, Chengyuan; Ma, Lishuang; He, Jiaojiao; Xiang, Junfeng; Deng, Xuebin; Wang, Ying; Chen, Xuebo; Jiang, Hua; Journal of the American Chemical Society 138 (2016) 15849–15852; doi:10.1021/jacs.6b10816

data_4131205
_publ_section_title
;
 Flexible, Linear Chains Act as Baffles To Inhibit the Intramolecular
 Rotation of Molecular Turnstiles.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15849
_journal_page_last               15852
_journal_paper_doi               10.1021/jacs.6b10816
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C50 H44 Cl2 N2 O6 Pd'
_chemical_formula_sum            'C50 H44 Cl2 N2 O6 Pd'
_chemical_formula_weight         946.17
_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             2016-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                94.504(2)
_cell_angle_beta                 99.812(2)
_cell_angle_gamma                109.967(3)
_cell_formula_units_Z            2
_cell_length_a                   8.9976(3)
_cell_length_b                   12.5054(4)
_cell_length_c                   24.0168(5)
_cell_measurement_reflns_used    11508
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.0120
_cell_measurement_theta_min      4.9370
_cell_volume                     2475.32(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      1.00  35.00   1.00    5.00    --  -41.49  77.00  30.00   34
  2  \w    -69.00 -30.00   1.00    5.00    --  -41.49  77.00  30.00   39
  3  \w      2.00  66.00   1.00    5.00    --   41.49 -99.00-150.00   64
  4  \w     91.00 120.00   1.00   15.00    --  107.19-125.00 -60.00   29
  5  \w     40.00 119.00   1.00   15.00    --  107.19 -30.00-180.00   79
  6  \w     87.00 119.00   1.00   15.00    --  107.19  45.00 -30.00   32
  7  \w    142.00 178.00   1.00   15.00    --  107.19  45.00   0.00   36
  8  \w    146.00 176.00   1.00   15.00    --  107.19  45.00 -30.00   30
  9  \w    141.00 174.00   1.00   15.00    --  107.19 125.00-180.00   33
 10  \w     96.00 121.00   1.00   15.00    --  107.19 125.00-180.00   25
 11  \w     94.00 153.00   1.00   15.00    --  107.19 125.00 -90.00   59
 12  \w     30.00  89.00   1.00   15.00    --  107.19 -94.00   0.00   59
 13  \w     36.00 107.00   1.00   15.00    --  107.19 -94.00 120.00   71
 14  \w    -97.00 -71.00   1.00    5.00    --  -41.49-139.00  31.00   26
 15  \w   -115.00 -16.00   1.00    5.00    --  -41.49 -57.00   0.00   99
 16  \w   -114.00 -23.00   1.00    5.00    --  -41.74 -37.00  60.00   91
 17  \w    -94.00  -4.00   1.00    5.00    --  -41.74 125.00-120.00   90
 18  \w     -5.00  21.00   1.00    5.00    --  -41.74  57.00 150.00   26
 19  \w    -65.00 -39.00   1.00    5.00    --  -41.74  57.00 150.00   26
 20  \w     47.00  85.00   1.00   15.00    --  107.19 -94.00 -60.00   38
 21  \w     44.00  70.00   1.00   15.00    --  107.19 -30.00  30.00   26
 22  \w     36.00 109.00   1.00   15.00    --  107.19 -94.00-150.00   73
 23  \w     70.00 131.00   1.00   15.00    --  107.19 -45.00 -60.00   61
 24  \w     78.00 105.00   1.00   15.00    --  107.19 -94.00  30.00   27
 25  \w     94.00 120.00   1.00   15.00    --  107.19-125.00  60.00   26
 26  \w     47.00  73.00   1.00   15.00    --  107.19 -61.00 150.00   26
 27  \w     87.00 115.00   1.00   15.00    --  107.19 -61.00 150.00   28
 28  \w    114.00 140.00   1.00   15.00    --  107.19  45.00 120.00   26
 29  \w    148.00 173.00   1.00   15.00    --  107.19  45.00 120.00   25
 30  \w    103.00 130.00   1.00   15.00    --  107.19 -30.00  30.00   27
 31  \w    106.00 158.00   1.00   15.00    --  107.19 -15.00 -60.00   52
 32  \w     28.00  79.00   1.00   15.00    --  107.19 -15.00 -60.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1382026000
_diffrn_orient_matrix_UB_12      -0.1175411000
_diffrn_orient_matrix_UB_13      -0.0074643000
_diffrn_orient_matrix_UB_21      -0.1197170000
_diffrn_orient_matrix_UB_22      0.0612071000
_diffrn_orient_matrix_UB_23      0.0065890000
_diffrn_orient_matrix_UB_31      -0.0359488000
_diffrn_orient_matrix_UB_32      -0.0001067000
_diffrn_orient_matrix_UB_33      -0.0650612000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20780
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.313
_diffrn_reflns_theta_min         3.777
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.991
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         9669
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0624
_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^)+(0.1012P)^2^+5.4690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8579
_reflns_number_total             9669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10816_si_002.cif
_cod_data_source_block           20160322a_sq
_cod_original_cell_volume        2475.30(14)
_cod_database_code               4131205
_chemical_oxdiff_formula         C1H1N1O1Pd
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.309
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C39, C39'}
3. Restrained distances
 O4-C46
 1.44 with sigma of 0.02
 C42-C43 = C43-C44 = C46-C47
 1.53 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C39) \\sim Ueq, Uanis(C39') \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C40')
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq,
Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40) = Uanis(C40')
Uanis(C39) = Uanis(C39')
Uanis(C49) = Uanis(C49') = Uanis(C50) = Uanis(C50')
5. Others
 Sof(H38C)=Sof(H38D)=Sof(C39')=Sof(H39C)=Sof(H39D)=Sof(C40')=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=FVAR(1)
 Sof(C49')=Sof(H49C)=Sof(H49D)=Sof(C50')=Sof(H50D)=Sof(H50E)=Sof(H50F)=1-FVAR(2)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C38(H38C,H38D), C39(H39A,H39B), C39'(H39C,
 H39D), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C46(H46A,H46B),
 C49(H49A,H49B), C49'(H49C,H49D)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12), C18(H18),
 C21(H21), C25(H25), C26(H26), C28(H28), C33(H33), C34(H34), C35(H35), C36(H36)
6.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C40'(H40D,H40E,H40F), C44(H44A,H44B,H44C), C47(H47A,H47B,
 H47C), C50(H50A,H50B,H50C), C50'(H50D,H50E,H50F)
;
_shelx_res_checksum              4028
_shelx_hkl_checksum              55969
_shelx_fab_checksum              42644
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.724
_oxdiff_exptl_absorpt_empirical_full_min 0.618