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_4133339
_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
'C67 H80 N6 O2 Zn, 2(Cl O4), 1.67(C2 H3 N), 0.25(O)'
_chemical_formula_sum            'C70.33 H85 Cl2 N7.66 O10.25 Zn'
_chemical_formula_weight         1337.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-16
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5497)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.984(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5821(3)
_cell_length_b                   19.5966(3)
_cell_length_c                   34.0945(6)
_cell_measurement_reflns_used    43042
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.9270
_cell_measurement_theta_min      1.9690
_cell_volume                     13992.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      100.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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    -98.00  11.00   0.50   15.00    --  -11.50 -57.00 120.00  218
  2  \w    -97.00 -44.00   0.50   15.00    --  -11.50 -57.00-180.00  106
  3  \w    -21.00   5.00   0.50   15.00    --  -11.50 -57.00-180.00   52
  4  \w    -49.00  23.00   0.50   15.00    --  -11.50  70.00 -60.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0123508000
_diffrn_orient_matrix_UB_12      0.0330109000
_diffrn_orient_matrix_UB_13      -0.0057858000
_diffrn_orient_matrix_UB_21      0.0073768000
_diffrn_orient_matrix_UB_22      0.0100271000
_diffrn_orient_matrix_UB_23      0.0206010000
_diffrn_orient_matrix_UB_31      0.0306664000
_diffrn_orient_matrix_UB_32      0.0108313000
_diffrn_orient_matrix_UB_33      -0.0015670000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            88346
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             5653
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.642
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1678
_refine_ls_number_reflns         27480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0875P)^2^+30.1451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1786
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22915
_reflns_number_total             27480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_008.cif
_cod_data_source_block           5-Zn(II)
_cod_database_code               4133339
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C70 H85 Cl2 N8 O10 Zn'
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.867
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Others
 Fixed Sof: N401(0.33) C401(0.33) C402(0.33) H40A(0.33) H40B(0.33) H40C(0.33)
 C501(0.6) C502(0.6) H50A(0.6) H50B(0.6) H50C(0.6) C503(0.4) C504(0.4)
 H50D(0.4) H50E(0.4) H50F(0.4) O201(0.5)
3.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), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,H11H), C120(H12C,
 H12D), C121(H12E,H12F), C122(H12G,H12H), C123(H12I,H12J), C130(H13C,H13D),
 C131(H13E,H13F), C132(H13G,H13H)
3.b Aromatic/amide H refined with riding coordinates:
 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), C33(H33), C36(H36), C37(H37),
  C38(H38), C41(H41), C43(H43), C45(H45), C55(H55), C57(H57), C59(H59),
 C102(H102), C103(H103), C104(H104), C107(H107), C108(H108), C109(H109),
 C115(H115), C116(H116), C118(H118), C119(H119), C125(H125), C126(H126),
 C128(H128), C129(H129), C133(H133), C136(H136), C137(H137), C138(H138),
 C141(H141), C143(H143), C145(H145), C155(H155), C157(H157), C159(H159)
3.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), C147(H14A,H14B,H14C), C148(H14D,H14E,H14F), C149(H14G,
 H14H,H14I), C151(H15A,H15B,H15C), C152(H15D,H15E,H15F), C153(H15G,H15H,H15I),
 C161(H16A,H16B,H16C), C162(H16D,H16E,H16F), C163(H16G,H16H,H16I), C165(H16J,
 H16K,H16L), C166(H16M,H16N,H16O), C167(H16P,H16Q,H16R), C202(H20C,H20D,H20E),
 C302(H30C,H30D,H30E), C402(H40A,H40B,H40C), C502(H50A,H50B,H50C), C504(H50D,
 H50E,H50F)
;
_shelx_res_checksum              98421
_shelx_hkl_checksum              58596
_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 1.263
_oxdiff_exptl_absorpt_empirical_full_min 0.826