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_1556902
_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         'C65 H76 N6 O6 Pt, F6 Sb [F6 Sb]'
_chemical_formula_sum            'C65 H76 F6 N6 O6 Pt Sb'
_chemical_formula_weight         1468.15
_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     iterative
_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                101.2515(11)
_cell_angle_beta                 102.1438(10)
_cell_angle_gamma                103.7234(10)
_cell_formula_units_Z            2
_cell_length_a                   11.78747(13)
_cell_length_b                   15.5279(2)
_cell_length_c                   22.4447(3)
_cell_measurement_reflns_used    55633
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7600
_cell_measurement_theta_min      2.1980
_cell_volume                     3769.49(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 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 0.998
_diffrn_measured_fraction_theta_max 0.916
_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    -35.00  71.00   1.00   10.00    --  -19.00  72.00-120.00  106
  2  \w    -78.00  20.00   1.00   10.00    --  -19.00 -72.00 120.00   98
  3  \w    -69.00  20.00   1.00   10.00    --  -19.00 -72.00 -60.00   89
  4  \w    -59.00  26.00   1.00   10.00    --  -19.00   0.00 -90.00   85
  5  \w    -30.00  -8.00   1.00   10.00    --  -19.00  72.00  60.00   22
  6  \w    -69.00  71.00   1.00   10.00    --  -19.00  18.00  90.00  140
  7  \w    -80.00  20.00   1.00   10.00    --  -19.00 -72.00 -90.00  100
  8  \w    -35.00  40.00   1.00   10.00    --  -19.00  54.00 150.00   75
  9  \w    -60.00  13.00   1.00   10.00    --  -19.00 -72.00  60.00   73
;
_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      -0.0022494000
_diffrn_orient_matrix_UB_12      0.0405977000
_diffrn_orient_matrix_UB_13      0.0200679000
_diffrn_orient_matrix_UB_21      0.0010059000
_diffrn_orient_matrix_UB_22      -0.0216297000
_diffrn_orient_matrix_UB_23      0.0250976000
_diffrn_orient_matrix_UB_31      0.0642722000
_diffrn_orient_matrix_UB_32      0.0158950000
_diffrn_orient_matrix_UB_33      0.0093291000
_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  0.0285
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            75959
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.810
_diffrn_reflns_theta_min         1.838
_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    2.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.607
_refine_diff_density_min         -2.878
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         21637
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0649P)^2^+9.6033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19979
_reflns_number_total             21637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05507j2.cif
_cod_data_source_block           ptnnc-ag-2
_cod_depositor_comments
;Adding full bibliography for 1556900--1556906.cif.

 Adding full bibliography for 1556900--1556906.cif.
;
_cod_original_cell_volume        3769.48(9)
_cod_database_code               1556902
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.895
_reflns_odcompleteness_completeness 91.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.74
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C78-C1 \\sim C78-C124
 with sigma of 0.02
 O8A-C1 \\sim O8-C124
 with sigma of 0.02
 O8-C0AA \\sim O8A-C0AB
 with sigma of 0.02
 C144-C0AA \\sim C2-C0AB
 with sigma of 0.02
 O15-C144 \\sim O15A-C2
 with sigma of 0.02
 O15-C127 \\sim O15A-C3
 with sigma of 0.02
 C3-C111 \\sim C127-C111
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C78, C124, C1, O8, O8A, C0AB, C0AA, C2, C144, O15, O15A, C127, C3, C111, O4,
 O41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(H78c)=Sof(H78d)=Sof(H11c)=Sof(H11d)=Sof(C1)=Sof(H1a)=Sof(H1b)=Sof(O8A)=
 Sof(C0AB)=Sof(H0Ac)=Sof(H0Ad)=Sof(C2)=Sof(H2a)=Sof(H2b)=Sof(O15A)=Sof(C3)=
 Sof(H3a)=Sof(H3b)=1-FVAR(1)
 Sof(O8)=Sof(O15)=Sof(H78a)=Sof(H78b)=Sof(H11a)=Sof(H11b)=Sof(C124)=Sof(H12d)=
 Sof(H12e)=Sof(C127)=Sof(H12f)=Sof(H12g)=Sof(C144)=Sof(H14a)=Sof(H14b)=
 Sof(C0AA)=Sof(H0Aa)=Sof(H0Ab)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C78(H78a,H78b), C78(H78c,H78d), C95(H95a,H95b), C111(H11a,H11b), C111(H11c,
 H11d), C116(H11e,H11f), C124(H12d,H12e), C127(H12f,H12g), C144(H14a,H14b),
 C0AA(H0Aa,H0Ab), C1(H1a,H1b), C0AB(H0Ac,H0Ad), C2(H2a,H2b), C3(H3a,H3b)
5.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C3AA(H3AA), C24(H24), C9(H9), C12(H12), C13(H13), C17(H17),
 C22(H22), C38(H38), C48(H48), C49(H49), C51(H51), C54(H54), C57(H57), C62(H62),
  C63(H63), C73(H73), C76(H76), C79(H79), C89(H89), C100(H100), C102(H102),
 C106(H106)
5.c Tetrahedral OH refined with riding coordinates:
 O3(H3)
5.d Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C44(H44a,H44b,H44c), C60(H60a,H60b,H60c), C65(H65a,H65b,
 H65c), C67(H67a,H67b,H67c), C82(H82a,H82b,H82c), C91(H91a,H91b,H91c),
 C108(H10a,H10b,H10c), C109(H10d,H10e,H10f), C118(H11g,H11h,H11i), C121(H12a,
 H12b,H12c), C139(H13a,H13b,H13c)
;
_shelx_res_checksum              88893
_shelx_fab_checksum              72850
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.870
_oxdiff_exptl_absorpt_empirical_full_min 0.410