Rotaxane-Based Transition Metal Complexes: Effect of the Mechanical Bond on Structure and Electronic Properties.
Cirulli, Martina; Kaur, Amanpreet; Lewis, James E. M.; Zhang, Zhihui; Kitchen, Jonathan A.; Goldup, Stephen M.; Roessler, Maxie M.; Journal of the American Chemical Society 141 (2019) 879–889; doi:10.1021/jacs.8b09715

data_4133347
_publ_section_title
;
 Rotaxane-Based Transition Metal Complexes: Effect of the Mechanical Bond
 on Structure and Electronic Properties.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              879
_journal_page_last               889
_journal_paper_doi               10.1021/jacs.8b09715
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C35 H46 N4, C32 H34 N2 O2'
_chemical_formula_sum            'C67 H80 N6 O2'
_chemical_formula_weight         1001.37
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.8300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0585(2)
_cell_length_b                   12.47470(10)
_cell_length_c                   25.7522(2)
_cell_measurement_reflns_used    26953
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.2870
_cell_measurement_theta_min      3.9210
_cell_volume                     5992.52(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9951
_diffrn_measured_fraction_theta_max 0.9783
_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    -76.00 -43.00   0.50    0.56    --    0.00   3.00 -45.00   66
  2  \w    -19.00   6.00   0.50    2.25    --    5.00   3.00 -45.00   50
  3  \w   -179.00 -37.00   0.50    2.25    --  -90.00   3.00 -45.00  284
  4  \w     38.00  64.00   0.50    0.56    --    0.00  60.00-180.00   52
  5  \w    -89.00  32.00   0.50    0.56    --    0.00  60.00-180.00  242
  6  \w   -179.00 -84.00   0.50    2.25    --  -90.00  57.00 -90.00  190
  7  \w   -172.00-145.00   0.50    2.25    --  -90.00  43.00   0.00   54
  8  \w   -135.00-109.00   0.50    2.25    --  -90.00  43.00   0.00   52
  9  \w    -66.00 -28.00   0.50    2.25    --  -90.00  43.00   0.00   76
 10  \w   -176.00 -13.00   0.50    2.25    --  -90.00  60.00 150.00  326
 11  \w   -169.00 -77.00   0.50    2.25    --  -90.00  60.00 120.00  184
 12  \w    -60.00 -35.00   0.50    2.25    --  -90.00  57.00 -90.00   50
 13  \w    -82.00 -25.00   0.50    2.25    --  -90.00  60.00-180.00  114
 14  \w   -116.00 -91.00   0.50    2.25    --  -90.00  43.00-150.00   50
 15  \w    -53.00 -16.00   0.50    2.25    --  -90.00  43.00-150.00   74
 16  \w   -177.00-151.00   0.50    2.25    --  -90.00  60.00  90.00   52
 17  \w   -166.00 -90.00   0.50    2.25    --  -90.00  60.00-180.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0661708000
_diffrn_orient_matrix_UB_12      0.0040990000
_diffrn_orient_matrix_UB_13      0.0458031000
_diffrn_orient_matrix_UB_21      0.0493403000
_diffrn_orient_matrix_UB_22      0.0040771000
_diffrn_orient_matrix_UB_23      -0.0404663000
_diffrn_orient_matrix_UB_31      -0.0037613000
_diffrn_orient_matrix_UB_32      0.1233029000
_diffrn_orient_matrix_UB_33      -0.0002206000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47039
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         67.000
_diffrn_reflns_theta_min         3.507
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
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    1.110
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10646
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0379P)^2^+2.8920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9820
_reflns_number_total             10646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_006.cif
_cod_data_source_block           5-Ligand
_cod_database_code               4133347
_chemical_oxdiff_formula         'C276 H324 N52 O8 '
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.895
_diffrn_oxdiff_ac3_digest_frames
;
015f1bbf93fa2cfdab840a95935c6e6c4200040317d
;
_diffrn_oxdiff_ac3_digest_hkl
;
010ad095e60b98b8833fae9b3afab9429049e8
;
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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. Restrained distances
 C53A-C51A
 2.5 with sigma of 0.005
 C52A-C50
 1.5 with sigma of 0.005
 C51A-C50
 1.5 with sigma of 0.005
 C50-C53A
 1.5 with sigma of 0.005
 C51A-C52A
 2.5 with sigma of 0.005
 C53A-C52A
 2.5 with sigma of 0.005
3. Others
 Fixed Sof: C51(0.75) H51A(0.75) H51B(0.75) H51C(0.75) C52(0.75) H52A(0.75)
 H52B(0.75) H52C(0.75) C53(0.75) H53A(0.75) H53B(0.75) H53C(0.75) C52A(0.25)
 H52D(0.25) H52E(0.25) H52F(0.25) C53A(0.25) H53D(0.25) H53E(0.25) H53F(0.25)
 C51A(0.25) H51D(0.25) H51E(0.25) H51F(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C36(H36), C37(H37), C38(H38), C41(H41), C43(H43), C45(H45),
 C55(H55), C57(H57), C59(H59), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9),
 C15(H15), C16(H16), C18(H18), C19(H19), C25(H25), C26(H26), C28(H28), C29(H29)
4.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C), C52A(H52D,H52E,H52F), C53A(H53D,H53E,H53F), C51A(H51D,
 H51E,H51F)
;
_shelx_shelxl_version_number     2018/1
_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 1.492
_oxdiff_exptl_absorpt_empirical_full_min 0.693