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_4133343
_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 N9 Ni O2, 1.5(Cl O4), 0.3(C4 H10 O), 0.4(H2 O)'
_chemical_formula_sum            'C70.2 H84.8 Cl1.5 N9 Ni O8.7'
_chemical_formula_weight         1305.75
_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             2018-04-16
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                79.3260(10)
_cell_angle_beta                 79.1510(10)
_cell_angle_gamma                85.4000(10)
_cell_formula_units_Z            4
_cell_length_a                   17.6574(2)
_cell_length_b                   19.5677(3)
_cell_length_c                   22.0939(3)
_cell_measurement_reflns_used    70306
_cell_measurement_temperature    124.27(10)
_cell_measurement_theta_max      30.2090
_cell_measurement_theta_min      3.0760
_cell_volume                     7359.47(18)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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_environment      N~2~
_diffrn_ambient_temperature      124.27(10)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9236
_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   -108.00  19.00   1.00    5.00    --  -19.10 -72.00-150.00  127
  2  \w   -108.00  19.00   1.00    5.00    --  -19.10 -72.00 -60.00  127
  3  \w   -108.00  15.00   1.00    5.00    --  -19.10 -37.00-150.00  123
  4  \w   -108.00  19.00   1.00    5.00    --  -19.10 -72.00  30.00  127
  5  \w    -53.00  70.00   1.00    5.00    --  -19.10  37.00-180.00  123
  6  \w   -108.00  16.00   1.00    5.00    --  -19.10 -57.00  60.00  124
  7  \w    -57.00  70.00   1.00    5.00    --  -19.10  72.00  90.00  127
  8  \w    -57.00 -32.00   1.00    5.00    --  -19.10  72.00-120.00   25
  9  \w    -57.00  70.00   1.00    5.00    --  -19.10  72.00 -30.00  127
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0294618000
_diffrn_orient_matrix_UB_12      0.0224763000
_diffrn_orient_matrix_UB_13      -0.0117338000
_diffrn_orient_matrix_UB_21      -0.0262653000
_diffrn_orient_matrix_UB_22      -0.0112913000
_diffrn_orient_matrix_UB_23      0.0279398000
_diffrn_orient_matrix_UB_31      0.0108965000
_diffrn_orient_matrix_UB_32      0.0270361000
_diffrn_orient_matrix_UB_33      0.0135452000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            198471
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.82
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68007
_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    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.645
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1703
_refine_ls_number_reflns         28866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0801P)^2^+7.2005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25227
_reflns_number_total             28866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_013.cif
_cod_data_source_block           6-Ni(II)
_cod_original_formula_sum        'C70.20 H84.80 Cl1.50 N9 Ni O8.70'
_cod_database_code               4133343
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.902
_reflns_odcompleteness_completeness 99.86
_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, All O(H,H) groups
2. Others
 Fixed Sof: O201(0.6) C170(0.5) C203(0.6) H20C(0.6) H20D(0.6) C67(0.6)
 H67A(0.6) H67B(0.6) H67C(0.6) C202(0.6) H20E(0.6) H20F(0.6) C69(0.6) H69A(0.6)
 H69B(0.6) H69C(0.6) C204(0.6) H20G(0.6) H20H(0.6) H20I(0.6) C201(0.6)
 H20J(0.6) H20K(0.6) H20L(0.6) C68(0.6) H68A(0.6) H68B(0.6) H68C(0.6) C173(0.5)
 H17A(0.5) H17B(0.5) H17C(0.5) C169(0.5) H16J(0.5) H16K(0.5) H16L(0.5)
 C167(0.5) H16M(0.5) H16N(0.5) H16O(0.5) C166(0.5) C172(0.5) H17D(0.5)
 H17E(0.5) H17F(0.5) C168(0.5) H16P(0.5) H16Q(0.5) H16R(0.5) C171(0.5)
 H17G(0.5) H17H(0.5) H17I(0.5) O302(0.4) H30C(0.4) H30D(0.4) O301(0.4)
 H30E(0.4) H30F(0.4) C71(0.4) H71A(0.4) H71B(0.4) H71C(0.4) C72(0.4) H72A(0.4)
 H72B(0.4) H72C(0.4) C70(0.4) H70A(0.4) H70B(0.4) H70C(0.4)
3.a Free rotating group:
 O302(H30C,H30D), O301(H30E,H30F)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13G,H13H), C132(H13A,H13B), C131(H13C,H13D), C111(H11A,H11B), C130(H13E,
 H13F), C11(H11G,H11H), C12(H12I,H12J), C20(H20A,H20B), C112(H11C,H11D),
 C21(H21A,H21B), C123(H12A,H12B), C113(H11E,H11F), C23(H23A,H23B), C31(H31A,
 H31B), C22(H22A,H22B), C122(H12C,H12D), C121(H12E,H12F), C120(H12G,H12H),
 C32(H32A,H32B), C30(H30A,H30B), C203(H20C,H20D), C202(H20E,H20F)
3.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C141(H141), C33(H33), C102(H102), C36(H36), C133(H133), C107(H107),
 C57(H57), C38(H38), C104(H104), C37(H37), C19(H19), C18(H18), C103(H103),
 C138(H138), C126(H126), C128(H128), C47(H47), C143(H143), C108(H108), C16(H16),
  C136(H136), C45(H45), C137(H137), C157(H157), C125(H125), C109(H109),
 C43(H43), C118(H118), C119(H119), C15(H15), C59(H59), C61(H61), C129(H129),
 C9(H9), C147(H147), C161(H161), C25(H25), C159(H159), C7(H7), C26(H26),
 C145(H145), C115(H115), C116(H116), C29(H29), C8(H8), C28(H28), C4(H4), C2(H2),
  C3(H3)
3.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C163(H16A,H16B,H16C), C54(H54A,H54B,H54C), C53(H53A,H53B,
 H53C), C164(H16D,H16E,H16F), C50(H50A,H50B,H50C), C150(H15A,H15B,H15C),
 C149(H14A,H14B,H14C), C151(H15D,H15E,H15F), C165(H16G,H16H,H16I), C51(H51A,
 H51B,H51C), C65(H65A,H65B,H65C), C64(H64A,H64B,H64C), C49(H49A,H49B,H49C),
 C153(H15G,H15H,H15I), C63(H63A,H63B,H63C), C154(H15J,H15K,H15L), C155(H15M,
 H15N,H15O), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C204(H20G,H20H,H20I),
 C201(H20J,H20K,H20L), C68(H68A,H68B,H68C), C173(H17A,H17B,H17C), C169(H16J,
 H16K,H16L), C167(H16M,H16N,H16O), C172(H17D,H17E,H17F), C168(H16P,H16Q,H16R),
 C171(H17G,H17H,H17I), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C70(H70A,H70B,
 H70C)
;
_shelx_fab_checksum              88385
_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 1.638
_oxdiff_exptl_absorpt_empirical_full_min 0.580