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_4133348
_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 N3 Ni O6, C4 H10 O, Cl0.25 O1.5, Cl0.75 O2.5'
_chemical_formula_sum            'C71 H90 Cl2 N3 Ni O11'
_chemical_formula_weight         1333.09
_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                104.093(2)
_cell_angle_beta                 95.803(2)
_cell_angle_gamma                101.189(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9467(3)
_cell_length_b                   15.0400(3)
_cell_length_c                   16.2204(3)
_cell_measurement_reflns_used    41342
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      32.2470
_cell_measurement_theta_min      3.2680
_cell_volume                     3426.92(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_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9336
_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  15.00   1.00    2.50    --  -22.90 -72.00 -30.00  127
  2  \w   -112.00  12.00   1.00    2.50    --  -22.90 -57.00  90.00  124
  3  \w   -112.00  15.00   1.00    2.50    --  -22.90 -72.00-150.00  127
  4  \w   -112.00  15.00   1.00    2.50    --  -22.90 -72.00  60.00  127
  5  \w    -56.00  66.00   1.00    2.50    --  -22.90  38.00  30.00  122
  6  \w   -112.00  15.00   1.00    2.50    --  -22.90 -72.00-120.00  127
  7  \w    -61.00  66.00   1.00    2.50    --  -22.90  72.00 -90.00  127
  8  \w    -61.00  66.00   1.00    2.50    --  -22.90  72.00  60.00  127
  9  \w    -61.00  66.00   1.00    2.50    --  -22.90  72.00 -30.00  127
 10  \w    -61.00  66.00   1.00    2.50    --  -22.90  72.00-180.00  127
 11  \w    -61.00  66.00   1.00    2.50    --  -22.90  72.00  30.00  127
 12  \w    -61.00  66.00   1.00    2.50    --  -22.90  72.00 150.00  127
 13  \w    -56.00  66.00   1.00    2.50    --  -22.90  38.00-180.00  122
 14  \w   -112.00 -87.00   1.00    2.50    --  -22.90 -38.00-120.00   25
 15  \w    -61.00  66.00   1.00    2.50    --  -22.90  72.00-120.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0381157000
_diffrn_orient_matrix_UB_12      0.0373652000
_diffrn_orient_matrix_UB_13      0.0022807000
_diffrn_orient_matrix_UB_21      -0.0208178000
_diffrn_orient_matrix_UB_22      0.0318079000
_diffrn_orient_matrix_UB_23      0.0272032000
_diffrn_orient_matrix_UB_31      0.0226331000
_diffrn_orient_matrix_UB_32      -0.0091890000
_diffrn_orient_matrix_UB_33      0.0365813000
_diffrn_radiation_collimation    0.3
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            60376
_diffrn_reflns_point_group_measured_fraction_full 0.998
_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         2.813
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67187
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         13462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0399P)^2^+1.9427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12554
_reflns_number_total             13462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09715_si_007.cif
_cod_data_source_block           5-Ni(II)
_cod_original_cell_volume        3426.91(12)
_cod_database_code               4133348
_chemical_oxdiff_formula         'Ni C69 H80 O16 N8 Cl3'
_chemical_oxdiff_usercomment     'JJ-DCM -tried at 200K'
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.920
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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: Cl31(0.25) O31(0.75) O32(0.25) O33(0.25) O34(0.25) Cl21(0.75)
 O21(0.75) O22(0.75) O23(0.75) O24(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), C72(H72A,H72B), C73(H73A,H73B)
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), C55(H55), C57(H57), C59(H59)
3.c Idealised Me refined as rotating group:
 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), C71(H71A,H71B,H71C), C74(H74A,H74B,H74C)
;
_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 1.704
_oxdiff_exptl_absorpt_empirical_full_min 0.695