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_4133336
_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
'0.5(C69 H81 Co N9 O2), 0.5(C69 H80 Co N9 O2), 1.5(Cl O4)'
_chemical_formula_sum            'C69 H80.5 Cl1.5 Co N9 O8'
_chemical_formula_weight         1276.02
_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             2018-04-18
_audit_creation_method
;
Olex2 1.2
(compiled Nov 22 2016 11:51:51 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                79.191(2)
_cell_angle_beta                 78.964(2)
_cell_angle_gamma                85.424(2)
_cell_formula_units_Z            4
_cell_length_a                   17.9110(4)
_cell_length_b                   19.5002(4)
_cell_length_c                   21.7320(5)
_cell_measurement_reflns_used    25446
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.8970
_cell_measurement_theta_min      2.9190
_cell_volume                     7310.2(3)
_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 0.9970
_diffrn_measured_fraction_theta_max 0.8756
_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    -51.00   1.00   1.00   34.53    --  -14.50 -57.00-150.00   52
  2  \w    -50.00  71.00   1.00   34.53    --  -14.50  72.00 120.00  121
  3  \w    -80.00 -35.00   1.00   34.53    --  -14.50 -57.00   0.00   45
  4  \w    -63.00  11.00   1.00   34.53    --  -14.50 -72.00-180.00   74
  5  \w    -89.00  21.00   1.00   34.53    --  -14.50 -72.00 -30.00  110
  6  \w    -46.00  19.00   1.00   34.53    --  -14.50  37.00 120.00   65
  7  \w     47.00  74.00   1.00   34.53    --  -14.50  37.00 120.00   27
  8  \w    -91.00 -57.00   1.00   34.53    --  -14.50 -57.00-150.00   34
;
_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      -0.0192405000
_diffrn_orient_matrix_UB_12      0.0176142000
_diffrn_orient_matrix_UB_13      0.0246479000
_diffrn_orient_matrix_UB_21      -0.0112723000
_diffrn_orient_matrix_UB_22      0.0276533000
_diffrn_orient_matrix_UB_23      -0.0230813000
_diffrn_orient_matrix_UB_31      -0.0336754000
_diffrn_orient_matrix_UB_32      -0.0172965000
_diffrn_orient_matrix_UB_33      0.0009454000
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            91166
_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         28.93
_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    0.345
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64269
_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    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1601
_refine_ls_number_reflns         25700
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0806
_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^)+(0.1067P)^2^+5.5738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2039
_refine_ls_wR_factor_ref         0.2321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16596
_reflns_number_total             25700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_009.cif
_cod_data_source_block           6-Co(II)
_cod_original_formula_sum        'C69 H80.50 Cl1.50 Co N9 O8'
_cod_database_code               4133336
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.944
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H,H,H,H) groups
2. Restrained distances
 C57-C56
 1.5 with sigma of 0.01
 C152-C154
 1.5 with sigma of 0.01
 C58-C54
 2.5 with sigma of 0.01
 C52-C58
 1.5 with sigma of 0.01
 C52-C54
 1.5 with sigma of 0.01
3. Others
 Fixed Sof: C153(0.5) H15G(0.5) H15H(0.5) H15I(0.5) C155(0.5) H15J(0.5)
 H15K(0.5) H15L(0.5) C157(0.5) H15M(0.5) H15N(0.5) H15O(0.5) C170(0.65)
 H17A(0.65) H17B(0.65) H17C(0.65) C172(0.65) H17D(0.65) H17E(0.65) H17F(0.65)
 C174(0.65) H17G(0.65) H17H(0.65) H17I(0.65) C154(0.5) H15P(0.5) H15Q(0.5)
 H15R(0.5) C156(0.5) H15S(0.5) H15T(0.5) H15U(0.5) C158(0.5) H15V(0.5)
 H15W(0.5) H15X(0.5) C171(0.35) H17J(0.35) H17K(0.35) H17L(0.35) C173(0.35)
 H17M(0.35) H17N(0.35) H17O(0.35) C175(0.35) H17P(0.35) H17Q(0.35) H17R(0.35)
 H53A(0.5) H53B(0.5) H53C(0.5) H53D(0.5) H53E(0.5) H53F(0.5) C52(0.5) C54(0.5)
 H54A(0.5) H54B(0.5) H54C(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C55(0.5)
 H55A(0.5) H55B(0.5) H55C(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5) C57(0.5)
4.a 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), C11(H11G,H11H), C12(H12I,H12J), C13(H13G,H13H), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C30(H30A,H30B), C31(H31A,H31B),
 C32(H32A,H32B)
4.b Me refined with riding coordinates:
 C53(H53A,H53B,H53C), C53(H53D,H53E,H53F)
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), C125(H125), C126(H126),
 C128(H128), C129(H129), C133(H133), C136(H136), C137(H137), C138(H138),
 C141(H141), C143(H143), C145(H145), C147(H147), C160(H160), C162(H162),
 C164(H164), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16),
  C18(H18), C19(H19), C20(H20), C25(H25), C26(H26), C28(H28), C29(H29),
 C33(H33), C36(H36), C37(H37), C38(H38), C41(H41), C43(H43), C45(H45), C47(H47),
  C60(H60), C62(H62), C64(H64)
4.d Idealised Me refined as rotating group:
 C149(H14A,H14B,H14C), C150(H15A,H15B,H15C), C151(H15D,H15E,H15F), C166(H16A,
 H16B,H16C), C167(H16D,H16E,H16F), C168(H16G,H16H,H16I), C153(H15G,H15H,H15I),
 C155(H15J,H15K,H15L), C157(H15M,H15N,H15O), C170(H17A,H17B,H17C), C172(H17D,
 H17E,H17F), C174(H17G,H17H,H17I), C154(H15P,H15Q,H15R), C156(H15S,H15T,H15U),
 C158(H15V,H15W,H15X), C171(H17J,H17K,H17L), C173(H17M,H17N,H17O), C175(H17P,
 H17Q,H17R), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,
 H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C54(H54A,H54B,H54C), C58(H58A,
 H58B,H58C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C)
;
_shelx_fab_checksum              10377
_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 1.541
_oxdiff_exptl_absorpt_empirical_full_min 0.598