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_4133338
_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 H80 Cl Co N6 O6, Cl O4, 0.38(C4 H10 O)'
_chemical_formula_sum            'C68.5 H83.75 Cl2 Co N6 O10.38'
_chemical_formula_weight         1286.99
_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
_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                80.6174(10)
_cell_angle_beta                 78.6057(10)
_cell_angle_gamma                85.0442(11)
_cell_formula_units_Z            4
_cell_length_a                   14.16695(19)
_cell_length_b                   15.3447(2)
_cell_length_c                   33.0606(4)
_cell_measurement_reflns_used    62083
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.0840
_cell_measurement_theta_min      1.8740
_cell_volume                     6940.15(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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_detector                 'CCD plate'
_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    -52.00  75.00   0.50    5.00    --  -14.30  57.00 -90.00  254
  2  \w   -104.00  26.00   0.50    5.00    --  -14.30 -70.00  90.00  260
  3  \w    -55.00  75.00   0.50    5.00    --  -14.30  70.00-150.00  260
  4  \w   -104.00  26.00   0.50    5.00    --  -14.30 -70.00 -60.00  260
  5  \w   -104.00  23.00   0.50    5.00    --  -14.30 -57.00 120.00  254
  6  \w   -104.00  23.00   0.50    5.00    --  -14.30 -57.00 -30.00  254
  7  \w    -52.00 -19.00   0.50    5.00    --  -14.30  57.00 120.00   66
  8  \w    -52.00  75.00   0.50    5.00    --  -14.30  57.00  60.00  254
;
_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      0.0092038000
_diffrn_orient_matrix_UB_12      0.0119542000
_diffrn_orient_matrix_UB_13      -0.0220064000
_diffrn_orient_matrix_UB_21      -0.0414817000
_diffrn_orient_matrix_UB_22      -0.0215325000
_diffrn_orient_matrix_UB_23      -0.0011980000
_diffrn_orient_matrix_UB_31      -0.0284834000
_diffrn_orient_matrix_UB_32      0.0399424000
_diffrn_orient_matrix_UB_33      0.0020540000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            132749
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.706
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (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    1.232
_exptl_crystal_description       block
_exptl_crystal_F_000             2723
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.869
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1618
_refine_ls_number_reflns         24442
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0648P)^2^+11.3937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21569
_reflns_number_total             24442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_003.cif
_cod_data_source_block           5-Co(II)
_cod_original_cell_volume        6940.17(16)
_cod_original_formula_sum        'C68.50 H83.75 Cl2 Co N6 O10.38'
_cod_database_code               4133338
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C65 H85 C2 Co1 N6 O11 '
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.894
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.16
_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. Restrained distances
 Cl31-O35
 1.4 with sigma of 0.01
3. Others
 Fixed Sof: O33(0.75) O34(0.75) O35(0.25) O36(0.25) O201(0.75) C201(0.75)
 H20C(0.75) H20D(0.75) H20E(0.75) C202(0.75) H20F(0.75) H20G(0.75) C203(0.75)
 H20H(0.75) H20I(0.75) C204(0.75) H20J(0.75) H20K(0.75) H20L(0.75)
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), C20(H20A,
 H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C202(H20F,H20G), C203(H20H,H20I)
4.b 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), C155(H155), C157(H157), C159(H159), 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), C55(H55), C57(H57), C59(H59)
4.c Idealised Me refined as rotating group:
 C147(H14A,H14B,H14C), C148(H14D,H14E,H14F), C149(H14G,H14H,H14I), C151(H15A,
 H15B,H15C), C152(H15D,H15E,H15F), C153(H15G,H15H,H15I), C161(H16A,H16B,H16C),
 C162(H16D,H16E,H16F), C163(H16G,H16H,H16I), C165(H16J,H16K,H16L), C166(H16M,
 H16N,H16O), C167(H16P,H16Q,H16R), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,
 H53C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C201(H20C,H20D,H20E),
 C204(H20J,H20K,H20L)
;
_shelx_res_checksum              34181
_shelx_hkl_checksum              56526
_shelx_fab_checksum              58747
_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 1.362
_oxdiff_exptl_absorpt_empirical_full_min 0.839