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_4133342
_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
'1(C69 H81 Cu N9 O2), 0.25(C H4 O), 2(Cl O4), 0.5(H2 O)'
_chemical_formula_sum            'C69.25 H83 Cl2 Cu N9 O10.75'
_chemical_formula_weight         1347.88
_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   mixed
_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                79.4340(10)
_cell_angle_beta                 79.3540(10)
_cell_angle_gamma                85.8910(10)
_cell_formula_units_Z            4
_cell_length_a                   17.8219(2)
_cell_length_b                   19.5882(3)
_cell_length_c                   21.7632(3)
_cell_measurement_reflns_used    115781
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.3580
_cell_measurement_theta_min      3.1810
_cell_volume                     7334.52(18)
_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      100.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9478
_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    -40.00  74.00   1.00    5.00    --  -15.70  37.00   0.00  114
  2  \w   -105.00  18.00   1.00    5.00    --  -15.70 -72.00-150.00  123
  3  \w   -105.00  18.00   1.00    5.00    --  -15.70 -72.00  60.00  123
  4  \w    -40.00  74.00   1.00    5.00    --  -15.70  37.00-120.00  114
  5  \w   -105.00  14.00   1.00    5.00    --  -15.70 -57.00 -90.00  119
  6  \w    -45.00  74.00   1.00    5.00    --  -15.70  57.00-180.00  119
  7  \w   -105.00   9.00   1.00    5.00    --  -15.70 -37.00  30.00  114
  8  \w    -49.00  74.00   1.00    5.00    --  -15.70  72.00 -60.00  123
  9  \w    -49.00  74.00   1.00    5.00    --  -15.70  72.00 120.00  123
 10  \w    -49.00  74.00   1.00    5.00    --  -15.70  72.00-120.00  123
 11  \w    -49.00  74.00   1.00    5.00    --  -15.70  72.00  30.00  123
 12  \w    -49.00  74.00   1.00    5.00    --  -15.70  72.00-180.00  123
 13  \w    -49.00  74.00   1.00    5.00    --  -15.70  72.00  60.00  123
 14  \w   -105.00 -80.00   1.00    5.00    --  -15.70 -37.00 150.00   25
;
_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      -0.0029041000
_diffrn_orient_matrix_UB_12      0.0323461000
_diffrn_orient_matrix_UB_13      0.0106860000
_diffrn_orient_matrix_UB_21      -0.0042377000
_diffrn_orient_matrix_UB_22      0.0174703000
_diffrn_orient_matrix_UB_23      -0.0308040000
_diffrn_orient_matrix_UB_31      -0.0402004000
_diffrn_orient_matrix_UB_32      -0.0027254000
_diffrn_orient_matrix_UB_33      0.0084164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            425150
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         32.88
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61482
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             2842
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.447
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1776
_refine_ls_number_reflns         25803
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+29.0317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2157
_refine_ls_wR_factor_ref         0.2198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23607
_reflns_number_total             25803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_011.cif
_cod_data_source_block           6-Cu(II)
_cod_database_code               4133342
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.900
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C232-C101
 1.515 with sigma of 0.02
 C232-C231
 1.515 with sigma of 0.02
 C132-C101
 1.515 with sigma of 0.02
 C132-C131
 1.515 with sigma of 0.02
 O300-C301
 1.35 with sigma of 0.01
3. Others
 Fixed Sof: C124(0.7) C125(0.7) H125(0.7) C126(0.7) H126(0.7) C127(0.7)
 C128(0.7) H128(0.7) C129(0.7) H129(0.7) C130(0.7) H13A(0.7) H13B(0.7)
 C131(0.7) H13C(0.7) H13D(0.7) C132(0.7) H13E(0.7) H13F(0.7) C155(0.6)
 H15J(0.6) H15K(0.6) H15L(0.6) C157(0.6) H15M(0.6) H15N(0.6) H15O(0.6)
 C159(0.6) H15P(0.6) H15Q(0.6) H15R(0.6) C156(0.4) H15S(0.4) H15T(0.4)
 H15U(0.4) C158(0.4) H15V(0.4) H15W(0.4) H15X(0.4) C160(0.4) H16G(0.4)
 H16H(0.4) H16I(0.4) C224(0.3) C225(0.3) H225(0.3) C226(0.3) H226(0.3)
 C227(0.3) C228(0.3) H228(0.3) C229(0.3) H229(0.3) C230(0.3) H23A(0.3)
 H23B(0.3) C231(0.3) H23C(0.3) H23D(0.3) C232(0.3) H23E(0.3) H23F(0.3)
 O300(0.5) H300(0.5) C301(0.5) H30C(0.5) H30D(0.5) H30E(0.5) Cl51(0.5) O51(0.5)
 O52(0.5) O53(0.5) O54(0.5) Cl61(0.5) O61(0.5) O62(0.5) O63(0.5) O64(0.5)
4.a Free rotating group:
 O71(H71A,H71B)
4.b Secondary CH2 refined with riding coordinates:
 C111(H11A,H11B), C112(H11C,H11D), C113(H11E,H11F), C120(H12A,H12B), C121(H12C,
 H12D), C122(H12E,H12F), C123(H12G,H12H), C130(H13A,H13B), C131(H13C,H13D),
 C132(H13E,H13F), C230(H23A,H23B), C231(H23C,H23D), C232(H23E,H23F), C11(H11G,
 H11H), C12(H12I,H12J), C13(H13G,H13H), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23G,H23H), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C107(H107), C108(H108), C109(H109),
 C115(H115), C116(H116), C118(H118), C119(H119), C135(H135), C138(H138),
 C139(H139), C140(H140), C143(H143), C145(H145), C147(H147), C149(H149),
 C162(H162), C164(H164), C166(H166), C125(H125), C126(H126), C128(H128),
 C129(H129), C225(H225), C226(H226), C228(H228), C229(H229), 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), C47(H47), C57(H57), C59(H59), C61(H61)
4.d Idealised Me refined as rotating group:
 C151(H15A,H15B,H15C), C152(H15D,H15E,H15F), C153(H15G,H15H,H15I), C168(H16A,
 H16B,H16C), C169(H16D,H16E,H16F), C170(H17A,H17B,H17C), C172(H17D,H17E,H17F),
 C173(H17G,H17H,H17I), C174(H17J,H17K,H17L), C155(H15J,H15K,H15L), C157(H15M,
 H15N,H15O), C159(H15P,H15Q,H15R), C156(H15S,H15T,H15U), C158(H15V,H15W,H15X),
 C160(H16G,H16H,H16I), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C301(H30C,H30D,H30E)
4.e Idealised tetrahedral OH refined as rotating group:
 O300(H300)
;
_shelx_fab_checksum              67841
_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 2.018
_oxdiff_exptl_absorpt_empirical_full_min 0.524