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_1556904
_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         'C69 H85 Ag N6 O6 Pt, 2(F6 Sb)'
_chemical_formula_sum            'C69 H85 Ag F12 N6 O6 Pt Sb2'
_chemical_formula_weight         1868.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-24 deposited with the CCDC.	2020-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.791(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7462(4)
_cell_length_b                   15.4022(3)
_cell_length_c                   27.6759(5)
_cell_measurement_reflns_used    19763
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.9890
_cell_measurement_theta_min      3.2710
_cell_volume                     7726.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_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      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.982
_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    -89.00  89.00   0.50    4.00    --    0.00  60.00 150.00  356
  2  \w    -89.00  89.00   0.50    4.00    --    0.00   0.00-180.00  356
  3  \w   -179.00  -1.00   0.50   21.03    --  -90.00  60.00 149.36  356
  4  \w   -179.00  -1.00   0.50   21.03    --  -90.00  58.00-179.72  356
  5  \w   -179.00  -1.00   0.50   21.03    --  -90.00  59.00  57.22  356
  6  \w   -168.00 -58.00   0.50   21.03    --  -90.00  26.00-114.06  220
  7  \w   -168.00 -58.00   0.50   21.03    --  -90.00  26.00-114.06  220
  8  \w    -63.00 -38.00   0.50   21.03    --  -90.00  59.00 -81.43   50
  9  \w   -135.00 -92.00   0.50   21.03    --  -90.00   0.00-180.00   86
 10  \w   -178.00-152.00   0.50   21.03    --  -90.00  10.00  60.00   52
 11  \w   -129.00 -87.00   0.50   21.03    --  -90.00  10.00  60.00   84
 12  \w    -57.00  -2.00   0.50   21.03    --  -90.00  10.00  60.00  110
 13  \w   -115.00 -88.00   0.50   21.03    --  -90.00  60.00 -68.06   54
 14  \w    -75.00 -37.00   0.50   21.03    --  -90.00  60.00 -68.06   76
 15  \w   -179.00-106.00   0.50   21.03    --  -90.00  60.00  -0.18  146
 16  \w    -88.00 -12.00   0.50   21.03    --  -90.00  60.00  -0.18  152
 17  \w    -91.00 -64.00   0.50   21.03    --  -90.00  58.00 157.99   54
 18  \w    -63.00  -1.00   0.50   21.03    --  -90.00  58.00 157.99  124
 19  \w   -124.00 -97.00   0.50   21.03    --  -90.00  56.00  63.16   54
 20  \w    -50.00 -23.00   0.50   21.03    --  -90.00  56.00  63.16   54
 21  \w   -151.00-124.00   0.50   21.03    --  -90.00  56.00-144.16   54
 22  \w    -70.00 -32.00   0.50   21.03    --  -90.00  59.00-123.83   76
 23  \w   -178.00 -92.00   0.50   21.03    --  -90.00  59.00-123.83  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 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      -0.0679829000
_diffrn_orient_matrix_UB_12      -0.0122628000
_diffrn_orient_matrix_UB_13      0.0210066000
_diffrn_orient_matrix_UB_21      0.0486556000
_diffrn_orient_matrix_UB_22      0.0138125000
_diffrn_orient_matrix_UB_23      0.0534105000
_diffrn_orient_matrix_UB_31      -0.0152818000
_diffrn_orient_matrix_UB_32      0.0982414000
_diffrn_orient_matrix_UB_33      -0.0048641000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1181
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            84286
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.067
_diffrn_reflns_theta_min         2.572
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    11.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (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    1.607
_exptl_crystal_description       plate
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.334
_refine_diff_density_min         -2.148
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         14409
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+25.2864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9956
_reflns_number_total             14409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05507j2.cif
_cod_data_source_block           zzvii-pt+ag_dz
_cod_depositor_comments
;Adding full bibliography for 1556900--1556906.cif.

 Adding full bibliography for 1556900--1556906.cif.
;
_cod_database_code               1556904
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C69 H85 Ag F12 N6 O6 Pt Sb2'
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.207
_reflns_odcompleteness_completeness 98.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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
 C01M-C02J \\sim C01M-C1AA
 with sigma of 0.02
 C01M-C02M \\sim C01M-C2AA
 with sigma of 0.02
 C01M-C02P \\sim C01M-C0AA
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C02P, C2AA, C02M, C1AA, C02J, C01M, C0AA
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(C0AA)=Sof(H0Ab)=Sof(H0Ac)=Sof(H0Ad)=Sof(C1AA)=Sof(H1Ab)=Sof(H1Ac)=
 Sof(H1Ad)=Sof(C2AA)=Sof(H2Ab)=Sof(H2Ac)=Sof(H2Ad)=1-FVAR(1)
 Sof(C02J)=Sof(H02t)=Sof(H02u)=Sof(H02v)=Sof(C02M)=Sof(H02)=Sof(Ha)=Sof(Hb)=
 Sof(C02P)=Sof(H2aa)=Sof(Hf)=Sof(Hg)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C01D(H01b,H01d), C01O(H01f,H01j), C020(H02a,H02b), C023(H02c,H02d), C027(H02e,
 H02f), C029(H02j,H02k), C02A(H02l,H02m), C02B(H02n,H02o), C02L(H02z,H),
 C02O(H1aa,He)
5.b Me refined with riding coordinates:
 C02R(H4aa,Hj,Hk), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c)
5.c Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00K(H00K), C00L(H00L), C31(H31), C00R(H00R), C30(H30),
 C00W(H00W), C00Z(H00Z), C011(H011), C017(H017), C019(H019), C01A(H01A),
 C01C(H01C), C01E(H01E), C01G(H01G), C01H(H01H), C01I(H01I), C01K(H01K),
 C01P(H01P), C01T(H01T), C01X(H01X), C026(H026), C02E(H02s)
5.d Idealised Me refined as rotating group:
 C01W(H01l,H01m,H01n), C01Y(H01o,H01q,H01r), C028(H02g,H02h,H02i), C02D(H02p,
 H02q,H02r), C02J(H02t,H02u,H02v), C02K(H02w,H02x,H02y), C02M(H02,Ha,Hb),
 C02N(H0aa,Hc,Hd), C02P(H2aa,Hf,Hg), C02Q(H3aa,Hh,Hi), C1(H1a,H1b,H1c),
 C0AA(H0Ab,H0Ac,H0Ad), C1AA(H1Ab,H1Ac,H1Ad), C2AA(H2Ab,H2Ac,H2Ad)
;
_shelx_res_checksum              89023
_shelx_fab_checksum              31621
_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_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 7.828
_oxdiff_exptl_absorpt_empirical_full_min 0.248