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_4133340
_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 H79 Cu N6 O2, F6 P'
_chemical_formula_sum            'C67 H79 Cu F6 N6 O2 P'
_chemical_formula_weight         1208.87
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-14
_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                 109.448(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3429(3)
_cell_length_b                   29.8447(5)
_cell_length_c                   16.0649(3)
_cell_measurement_reflns_used    61475
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.7880
_cell_measurement_theta_min      1.9310
_cell_volume                     6936.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (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_measured_fraction_theta_full 1.000
_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   -100.00  23.00   0.50   32.00    --  -11.50 -57.00 -90.00  246
  2  \w   -100.00  77.00   0.50   32.00    --  -11.50 -19.00 150.00  354
  3  \w   -100.00  26.00   0.50   32.00    --  -11.50 -70.00 -60.00  252
  4  \w   -100.00  26.00   0.50   32.00    --  -11.50 -70.00-180.00  252
  5  \w   -100.00  23.00   0.50   32.00    --  -11.50 -57.00  30.00  246
  6  \w    -58.00 -33.00   0.50   32.00    --  -11.50  38.00  60.00   50
  7  \w    -49.00  77.00   0.50   32.00    --  -11.50  70.00-120.00  252
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            133987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.730
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
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    1.158
_exptl_crystal_description       plate
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         12214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0961
_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^)+(0.0499P)^2^+23.8807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11101
_reflns_number_total             12214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_004.cif
_cod_data_source_block           5-Cu(I)
_cod_database_code               4133340
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.925
_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, All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) H30D(0.5) H56(0.5) H56A(0.5)
 H66A(0.5) H66B(0.5) H66C(0.5) H66D(0.5) H66E(0.5) H66F(0.5) H68A(0.5)
 H68B(0.5) H68C(0.5) H68D(0.5) H68E(0.5) H68F(0.5) C57(0.5) C58(0.5) H58(0.5)
 C59(0.5) C60(0.5) H60(0.5) C61(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
 C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5)
 C69(0.5) H69(0.5) C70(0.5) H70(0.5) C71(0.5) H71(0.5) C72(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) C74(0.5) H74A(0.5) H74B(0.5) C75(0.5) H75A(0.5) H75B(0.5)
 C76(0.5) C77(0.5) H77(0.5) C78(0.5) H78(0.5) C79(0.5) C80(0.5) H80(0.5)
 C81(0.5) H81(0.5) C82(0.5) H82A(0.5) H82B(0.5) C83(0.5) H83A(0.5) H83B(0.5)
 C92(0.5) C93(0.5) H93A(0.5) H93B(0.5) H93C(0.5) C7(0.5) H7(0.5) C8(0.5)
 H8(0.5) C9(0.5) H9(0.5) C10(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5)
 H12A(0.5) H12B(0.5) C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) C15(0.5) H15(0.5)
 C16(0.5) H16(0.5) C17(0.5) C18(0.5) H18(0.5) C19(0.5) H19(0.5) C31(0.5)
 H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5) C65(0.5) C67(0.5) H67A(0.5)
 H67B(0.5) H67C(0.5) C84(0.5) C85(0.5) H85(0.5) C86(0.5) C87(0.5) H87(0.5)
 C88(0.5) C89(0.5) H89A(0.5) H89B(0.5) H89C(0.5) C90(0.5) H90A(0.5) H90B(0.5)
 H90C(0.5) C91(0.5) H91A(0.5) H91B(0.5) H91C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C30(H30A,H30B), C30(H30C,
 H30D), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C82(H82A,H82B),
 C83(H83A,H83B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C31(H31A,H31B),
  C32(H32A,H32B)
3.b Me refined with riding coordinates:
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29),
 C34(H34), C37(H37), C38(H38), C39(H39), C42(H42), C44(H44), C46(H46), C56(H56),
  C56(H56A), C58(H58), C60(H60), C69(H69), C70(H70), C71(H71), C77(H77),
 C78(H78), C80(H80), C81(H81), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16),
 C18(H18), C19(H19), C85(H85), C87(H87)
3.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C66(H66D,H66E,H66F), C68(H68A,
 H68B,H68C), C68(H68D,H68E,H68F), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C), C93(H93A,H93B,H93C), C89(H89A,H89B,H89C), C90(H90A,H90B,
 H90C), C91(H91A,H91B,H91C)
;
_shelx_res_checksum              32221
_shelx_hkl_checksum              77073
_shelx_fab_checksum              57186
_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
;