Rotaxane PtII-complexes: mechanical bonding for chemically robust luminophores and stimuli responsive behaviour
Zhang, Zhihui; Tizzard, Graham J.; Williams, J. A. Gareth; Goldup, Stephen M.; Chemical Science 11 (2020) 1839–1847; doi:10.1039/C9SC05507J

data_1556905
_publ_section_title
;
 Rotaxane PtII-complexes: mechanical bonding for chemically robust
 luminophores and stimuli responsive behaviour
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              1839
_journal_page_last               1847
_journal_paper_doi               10.1039/C9SC05507J
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C60 H72 N5 O5 Pt, B F4'
_chemical_formula_sum            'C60 H72 B F4 N5 O5 Pt'
_chemical_formula_weight         1225.12
_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             2019-10-29
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.24 svn.r3677 for OlexSys, GUI svn.r5967)
;
_audit_update_record
;
2019-11-01 deposited with the CCDC.	2020-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                81.1180(10)
_cell_angle_beta                 76.0170(10)
_cell_angle_gamma                74.0980(10)
_cell_formula_units_Z            2
_cell_length_a                   12.23750(10)
_cell_length_b                   14.6363(2)
_cell_length_c                   18.2789(2)
_cell_measurement_reflns_used    53968
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1140
_cell_measurement_theta_min      2.2960
_cell_volume                     3041.70(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  68.00   1.00    5.00    --  -22.00   0.00-120.00  180
  2  \w    -70.00  17.00   1.00    5.00    --  -22.00 -72.00   0.00   87
  3  \w    -82.00   8.00   1.00    5.00    --  -22.00 -72.00-120.00   90
  4  \w    -36.00  68.00   1.00    5.00    --  -22.00  72.00 120.00  104
  5  \w    -60.00 -14.00   1.00    5.00    --  -22.00 -72.00-180.00   46
  6  \w    -22.00 -10.00   1.00    5.00    --  -22.00 -72.00 120.00   12
  7  \w   -112.00  68.00   1.00    5.00    --  -22.00   0.00   0.00  180
  8  \w    -70.00  17.00   1.00    5.00    --  -22.00 -72.00 -30.00   87
  9  \w    -85.00   9.00   1.00    5.00    --  -22.00 -72.00-150.00   94
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0438719000
_diffrn_orient_matrix_UB_12      0.0087477000
_diffrn_orient_matrix_UB_13      0.0332727000
_diffrn_orient_matrix_UB_21      0.0375691000
_diffrn_orient_matrix_UB_22      -0.0321248000
_diffrn_orient_matrix_UB_23      0.0217780000
_diffrn_orient_matrix_UB_31      0.0215207000
_diffrn_orient_matrix_UB_32      0.0381251000
_diffrn_orient_matrix_UB_33      0.0056758000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            70650
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.509
_diffrn_reflns_theta_min         2.307
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.368
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of MeCN and ether  by slow evaporation'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.033
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         18500
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+1.9727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17305
_reflns_number_total             18500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05507j2.cif
_cod_data_source_block           jl2016kzz0704z
_cod_depositor_comments
;Adding full bibliography for 1556900--1556906.cif.

 Adding full bibliography for 1556900--1556906.cif.
;
_cod_database_code               1556905
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H72 B F4 N5 O5 Pt'
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.649
_reflns_odcompleteness_completeness 99.54
_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. Restrained distances
 F4A-B1 \\sim F4B-B1
 with sigma of 0.02
 F1A-B1 \\sim F1B-B1
 with sigma of 0.02
 F2A-B1 \\sim F2B-B1
 with sigma of 0.02
 F3A-B1 \\sim F3B-B1
 with sigma of 0.02
 C57-C60A \\sim C57-C58B
 with sigma of 0.02
 C57-C58A \\sim C57-C59B
 with sigma of 0.02
 C57-C59A \\sim C57-C60B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C58B, C58A, C59B, C59A, C60B, C60A, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1B, F1A, F3A, F3B, F4B, F4A, F2B, F2A, B1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=FVAR(1)
 Sof(C58B)=Sof(H58D)=Sof(H58E)=Sof(H58F)=Sof(C59B)=Sof(H59D)=Sof(H59E)=
 Sof(H59F)=Sof(C60B)=Sof(H60D)=Sof(H60E)=Sof(H60F)=1-FVAR(2)
 Sof(C58A)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59A)=Sof(H59A)=Sof(H59B)=
 Sof(H59C)=Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(H60C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C36(H36), C42(H42), C43(H43),
  C45(H45), C48(H48), C49(H49), C55(H55)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C54(H54A,H54B,H54C), C58A(H58A,H58B,H58C), C59A(H59A,H59B,H59C),
 C60A(H60A,H60B,H60C), C58B(H58D,H58E,H58F), C59B(H59D,H59E,H59F), C60B(H60D,
 H60E,H60F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13649
_shelx_fab_checksum              30880
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id Pt(I)BF4
_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 1.496
_oxdiff_exptl_absorpt_empirical_full_min 0.752