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_1556906
_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         'C67 H77 Ag N7 O5 Pt, 5(F3 Sb0.5)'
_chemical_formula_sum            'C67 H77 Ag F15 N7 O5 Pt Sb2.5'
_chemical_formula_weight         1952.69
_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             2019-06-20
_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                88.810(3)
_cell_angle_beta                 89.789(3)
_cell_angle_gamma                83.438(3)
_cell_formula_units_Z            2
_cell_length_a                   13.0371(5)
_cell_length_b                   18.3984(8)
_cell_length_c                   18.4639(8)
_cell_measurement_reflns_used    17360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.4120
_cell_measurement_theta_min      1.9200
_cell_volume                     4398.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (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(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -97.00  29.00   0.50   10.00    --   -7.70 -70.00 -60.00  252
  2  \w    -97.00  26.00   0.50   10.00    --   -7.70 -57.00 120.00  246
  3  \w    -75.00  82.00   0.50   10.00    --   -7.70  19.00 -30.00  314
  4  \w    -75.00  82.00   0.50   10.00    --   -7.70  19.00 150.00  314
  5  \w    -41.00 -16.00   0.50   10.00    --   -7.70  57.00  30.00   50
  6  \w    -44.00  82.00   0.50   10.00    --   -7.70  70.00-150.00  252
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type  Ros_HyPix
_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      -0.0411462000
_diffrn_orient_matrix_UB_12      0.0164259000
_diffrn_orient_matrix_UB_13      0.0215037000
_diffrn_orient_matrix_UB_21      -0.0133337000
_diffrn_orient_matrix_UB_22      0.0263102000
_diffrn_orient_matrix_UB_23      -0.0280148000
_diffrn_orient_matrix_UB_31      -0.0335918000
_diffrn_orient_matrix_UB_32      -0.0233351000
_diffrn_orient_matrix_UB_33      -0.0151398000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            85505
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.116
_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    2.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1911
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         6.968
_refine_diff_density_min         -2.474
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         15515
_refine_ls_number_restraints     1177
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0944P)^2^+27.3760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12452
_reflns_number_total             15515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05507j2.cif
_cod_data_source_block           20180519zz1
_cod_depositor_comments
;Adding full bibliography for 1556900--1556906.cif.

 Adding full bibliography for 1556900--1556906.cif.
;
_cod_original_formula_sum        'C67 H77 Ag F15 N7 O5 Pt Sb2.50'
_cod_database_code               1556906
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pt C60 H N O Ag'
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.505
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 O01H-C4 \\sim O01H-C4A
 with sigma of 0.02
 O01Z-C7 \\sim O01Z-C7A
 with sigma of 0.02
 C4-C7 \\sim C4A-C7A
 with sigma of 0.02
 O01H-C7 \\sim O01H-C7A
 with sigma of 0.04
 O01Z-C4 \\sim O01Z-C4A
 with sigma of 0.04
 O00Z-C16 \\sim O00Z-C16A
 with sigma of 0.02
 O01H-C19 \\sim O01H-C19A
 with sigma of 0.02
 C16-C19 \\sim C16A-C19A
 with sigma of 0.02
 O00Z-C19 \\sim O00Z-C19A
 with sigma of 0.04
 O01H-C16 \\sim O01H-C16A
 with sigma of 0.04
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 C16, C19, O01H, C4, C7, O01Z, C02O
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=1-FVAR(1)
 Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(C7)=Sof(H7a)=Sof(H7b)=FVAR(1)
 Sof(C19A)=Sof(H19c)=Sof(H19d)=Sof(C16A)=Sof(H16c)=Sof(H16d)=1-FVAR(2)
 Sof(C16)=Sof(H16a)=Sof(H16b)=Sof(C19)=Sof(H19a)=Sof(H19b)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C027(H02m,H02n), C029(H02o,H02p), C02A(H02q,H02r), C16(H16a,H16b), C19(H19a,
 H19b), C4(H4a,H4b), C7(H7a,H7b), C4A(H4Aa,H4Ab), C7A(H7Aa,H7Ab), C19A(H19c,
 H19d), C16A(H16c,H16d)
6.b Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00N(H00N), C00W(H00W), C00Y(H00Y), C013(H013), C014(H014),
 C015(H015), C016(H016), C018(H018), C01A(H01A), C01B(H01B), C01C(H01C),
 C01I(H01I), C01K(H01K), C01L(H01L), C01M(H01M), C01O(H01O), C01U(H01U),
 C01V(H01V), C026(H026), C02O(H1aa), C0AA(H0Ab), C2AA(H2AA), C6(H6)
6.c Idealised Me refined as rotating group:
 C01N(H01d,H01e,H01f), C01Q(H01g,H01h,H01j), C020(H02a,H02b,H02c), C022(H02d,
 H02e,H02f), C024(H02g,H02h,H02i), C025(H02j,H02k,H02l), C02C(H02s,H02t,H02u),
 C02D(H02v,H02w,H02x), C02G(H02y,H,Ha), C02I(H02z,Hb,Hc), C02J(H02,Hd,He),
 C02N(H0aa,Hf,Hg), C5(H5a,H5b,H5c)
;
_shelx_res_checksum              60996
_shelx_fab_checksum              44323
_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 1.629
_oxdiff_exptl_absorpt_empirical_full_min 0.615