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_4133341
_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         'C69 H81 Cu N9 O2, 0.25(C4 H10 O), F6 P'
_chemical_formula_sum            'C70 H83.5 Cu F6 N9 O2.25 P'
_chemical_formula_weight         1295.46
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-12
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                107.853(2)
_cell_angle_beta                 93.183(2)
_cell_angle_gamma                108.418(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4007(2)
_cell_length_b                   15.0780(3)
_cell_length_c                   22.0734(4)
_cell_measurement_reflns_used    27803
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.9540
_cell_measurement_theta_min      3.1270
_cell_volume                     3377.56(13)
_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 0.9983
_diffrn_measured_fraction_theta_max 0.9374
_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   -112.00  21.00   1.00   50.00    --  -22.20 -72.00  30.00  133
  2  \w   -112.00  21.00   1.00   50.00    --  -22.20 -72.00 -60.00  133
  3  \w   -112.00  21.00   1.00   50.00    --  -22.20 -72.00 150.00  133
  4  \w   -112.00  21.00   1.00   50.00    --  -22.20 -72.00   0.00  133
  5  \w    -67.00  67.00   1.00   50.00    --  -22.20  38.00 150.00  134
  6  \w   -112.00  22.00   1.00   50.00    --  -22.20 -38.00-180.00  134
  7  \w   -112.00  21.00   1.00   50.00    --  -22.20 -72.00-150.00  133
  8  \w    -66.00  44.00   1.00   50.00    --  -22.20  72.00  30.00  110
  9  \w    -66.00  67.00   1.00   50.00    --  -22.20  72.00 -90.00  133
;
_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      -0.0155635000
_diffrn_orient_matrix_UB_12      -0.0089954000
_diffrn_orient_matrix_UB_13      -0.0334242000
_diffrn_orient_matrix_UB_21      0.0381034000
_diffrn_orient_matrix_UB_22      0.0496734000
_diffrn_orient_matrix_UB_23      0.0045637000
_diffrn_orient_matrix_UB_31      0.0522678000
_diffrn_orient_matrix_UB_32      -0.0153598000
_diffrn_orient_matrix_UB_33      -0.0059232000
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70110
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.865
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82116
_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    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             1365
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         13273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0525P)^2^+4.1126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11733
_reflns_number_total             13273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_010.cif
_cod_data_source_block           6-Cu(I)
_cod_original_cell_volume        3377.55(12)
_cod_original_formula_sum        'C70 H83.50 Cu F6 N9 O2.25 P'
_cod_database_code               4133341
_chemical_oxdiff_usercomment     888/4
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.922
_reflns_odcompleteness_completeness 99.83
_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: O71(0.25) C70(0.25) H70A(0.25) H70B(0.25) H70C(0.25) C71(0.25)
 H71A(0.25) H71B(0.25) C72(0.25) H72A(0.25) H72B(0.25) C73(0.25) H73A(0.25)
 H73B(0.25) H73C(0.25)
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), C71(H71A,H71B), C72(H72A,H72B)
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), C47(H47), C57(H57), C59(H59), C61(H61)
3.c Idealised Me refined as rotating group:
 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), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C)
;
_shelx_res_checksum              59101
_shelx_hkl_checksum              87924
_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 1.830
_oxdiff_exptl_absorpt_empirical_full_min 0.665