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_1556900
_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         'C32 H49 Cl2 N3 O Pt S, C30 H30 N2 O5'
_chemical_formula_sum            'C62 H79 Cl2 N5 O6 Pt S'
_chemical_formula_weight         1288.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 106.494(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.7934(5)
_cell_length_b                   12.4321(3)
_cell_length_c                   39.1414(7)
_cell_measurement_reflns_used    13983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.3260
_cell_measurement_theta_min      3.8050
_cell_volume                     12501.4(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (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 (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 0.901
_diffrn_measured_fraction_theta_max 0.897
_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    -77.00  69.00   1.00   10.00    --  -17.00  15.00-150.00  146
  2  \w     52.00  59.00   1.00   10.00    --  -17.00  52.00-180.00    7
  3  \w   -179.00   0.00   1.00   10.00    --  -90.00  60.00   0.00  179
  4  \w   -179.00 -99.00   1.00   10.00    --  -90.00  45.00 120.00   80
  5  \w    -98.00 -47.00   1.00   10.00    --  -90.00  60.00-120.00   51
  6  \w   -159.00 -98.00   1.00   10.00    --  -90.00  30.00 120.00   61
  7  \w   -147.00 -82.00   1.00   10.00    --  -90.00  37.00 -60.00   65
  8  \w   -173.00-113.00   1.00   10.00    --  -90.00  45.00 -30.00   60
;
_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      -0.0410768000
_diffrn_orient_matrix_UB_12      0.0280344000
_diffrn_orient_matrix_UB_13      -0.0352202000
_diffrn_orient_matrix_UB_21      -0.0152707000
_diffrn_orient_matrix_UB_22      -0.1195949000
_diffrn_orient_matrix_UB_23      -0.0054166000
_diffrn_orient_matrix_UB_31      -0.0408834000
_diffrn_orient_matrix_UB_32      0.0165394000
_diffrn_orient_matrix_UB_33      0.0203786000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.901
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            24565
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.441
_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    5.706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (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    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.089
_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     776
_refine_ls_number_reflns         10265
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+3.9850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9484
_reflns_number_total             10265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05507j2.cif
_cod_data_source_block           2016jlzz1072dgty
_cod_depositor_comments
;Adding full bibliography for 1556900--1556906.cif.

 Adding full bibliography for 1556900--1556906.cif.
;
_cod_database_code               1556900
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H60 Cl S N10 Pt'
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.599
_reflns_odcompleteness_completeness 89.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
2. Restrained distances
 C53-C55A \\sim C53-C55B \\sim C53-C54A \\sim C53-C56B \\sim C53-C56A \\sim
C53-C54B
 with sigma of 0.02
 C54A-C55A \\sim C54A-C56A \\sim C55A-C56A \\sim C54B-C55B \\sim C54B-C56B
\\sim C55B-C56B
 with sigma of 0.04
 O1A-C20 \\sim O1B-C20 \\sim O2A-C25 \\sim O2B-C25 \\sim O2A-C24A \\sim
O2B-C24B \\sim O1A-C23A \\sim O1B-
 C23B
 with sigma of 0.02
 C23A-C24A \\sim C23B-C24B
 with sigma of 0.02
 O1A-C24A \\sim O1B-C24B \\sim O2A-C23A \\sim O2B-C23B
 with sigma of 0.04
 C20-C23A \\sim C20-C23B \\sim C25-C24A \\sim C25-C24B
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 C20, C25, O1A, O2A, C23A, C24A, O1B, O2B, C23B, C24B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56B, C55A, C55B, C56A, C54B, C54A, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C54B)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C55B)=Sof(H55D)=Sof(H55E)=
 Sof(H55F)=Sof(C56B)=Sof(H56D)=Sof(H56E)=Sof(H56F)=1-FVAR(1)
 Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C55A)=Sof(H55A)=Sof(H55B)=
 Sof(H55C)=Sof(C56A)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(1)
 Sof(H25C)=Sof(H25D)=Sof(O1B)=Sof(O2B)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=
 Sof(H24C)=Sof(H24D)=1-FVAR(2)
 Sof(H25A)=Sof(H25B)=Sof(O1A)=Sof(O2A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=
 Sof(H24A)=Sof(H24B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C25(H25C,H25D), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C23A(H23A,H23B), C24A(H24A,H24B),
 C23B(H23C,H23D), C24B(H24C,H24D)
5.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C34(H34), C36(H36), C45(H45), C48(H48), C50(H50), C52(H52), C2(H2),
 C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15),
  C18(H18), C19(H19), C21(H21), C22(H22)
5.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C58(H58A,H58B,H58C), C59(H59A,
 H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C54A(H54A,H54B,H54C), C55A(H55A,H55B,H55C), C56A(H56A,H56B,H56C), C54B(H54D,
 H54E,H54F), C55B(H55D,H55E,H55F), C56B(H56D,H56E,H56F)
;
_shelx_res_checksum              74260
_shelx_fab_checksum              63833
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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 3.818
_oxdiff_exptl_absorpt_empirical_full_min 0.233