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_1556903
_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 H75 N6 O5 Pt, B F4'
_chemical_formula_sum            'C66 H77 B F4 N8 O5 Pt'
_chemical_formula_weight         1344.25
_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     iterative
_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                90
_cell_angle_beta                 107.531(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7380(4)
_cell_length_b                   14.9289(3)
_cell_length_c                   21.8888(5)
_cell_measurement_reflns_used    20929
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.4010
_cell_measurement_theta_min      1.8110
_cell_volume                     6773.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_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 0.856
_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    -56.00  72.00   0.25    3.99    --  -17.30  65.00   0.00  512
  2  \w   -107.00  21.00   0.25    3.99    --  -17.30 -65.00-135.00  512
  3  \w   -107.00  20.00   0.25    3.99    --  -17.30 -57.00  90.00  508
  4  \w   -107.00 -78.00   0.25    3.99    --  -17.30 -57.00   0.00  116
  5  \w    -55.00  72.00   0.25    3.99    --  -17.30  57.00-180.00  508
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0237776000
_diffrn_orient_matrix_UB_12      -0.0138238000
_diffrn_orient_matrix_UB_13      -0.0284395000
_diffrn_orient_matrix_UB_21      -0.0215039000
_diffrn_orient_matrix_UB_22      0.0327504000
_diffrn_orient_matrix_UB_23      0.0051886000
_diffrn_orient_matrix_UB_31      0.0119857000
_diffrn_orient_matrix_UB_32      0.0315041000
_diffrn_orient_matrix_UB_33      -0.0178682000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            94830
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.003
_diffrn_reflns_theta_min         1.789
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.134
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.682
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         20137
_refine_ls_number_restraints     4407
_refine_ls_restrained_S_all      0.820
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16483
_reflns_number_total             20137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05507j2.cif
_cod_data_source_block           zzv-ptnnc
_cod_depositor_comments
;Adding full bibliography for 1556900--1556906.cif.

 Adding full bibliography for 1556900--1556906.cif.
;
_cod_database_code               1556903
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.815
_reflns_odcompleteness_completeness 99.96
_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. Uiso/Uaniso restraints and constraints
C7 \\sim C11 \\sim C5 \\sim C12 \\sim C8 \\sim C47 \\sim C9 \\sim C13 \\sim C10
\\sim C6 \\sim C48 \\sim C54 \\sim C3 \\sim C44 \\sim C4 \\sim C46 \\sim C57
\\sim C16 \\sim C20 \\sim C45 \\sim C2 \\sim C52 \\sim C18 \\sim C21 \\sim C17
\\sim C14 \\sim C51 \\sim C19 \\sim C1 \\sim C53 \\sim C15 \\sim C22 \\sim C58
\\sim C56 \\sim C36 \\sim C23 \\sim C49 \\sim C59 \\sim C50 \\sim C31 \\sim C55
\\sim C30 \\sim C66 \\sim C43 \\sim C24 \\sim C37 \\sim C61 \\sim C60 \\sim C38
\\sim C29 \\sim C32 \\sim C40 \\sim C39 \\sim C35 \\sim C62 \\sim C25 \\sim C27
\\sim C26 \\sim C33 \\sim C34 \\sim C63 \\sim C42 \\sim C41 \\sim C65 \\sim
C64: within 6.2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C62, C65
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C23(H23a,H23b), C31(H31a,H31b), C30(H30a,H30b), C24(H24a,H24b), C29(H29a,
 H29b), C25(H25a,H25b), C27(H27a,H27b), C26(H26a,H26b)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C13(H13), C10(H10), C54(H54), C3(H3), C44(H44), C4(H4),
 C46(H46), C20(H20), C2(H2), C18(H18), C21(H21), C14(H14), C51(H51), C19(H19),
 C15(H15), C49(H49), C50(H50), C55(H55), C43(H43), C37(H37), C61(H61)
4.c Idealised Me refined as rotating group:
 C58(H58a,H58b,H58c), C59(H59a,H59b,H59c), C60(H60a,H60b,H60c), C32(H32a,H32b,
 H32c), C40(H40a,H40b,H40c), C33(H33a,H33b,H33c), C34(H34a,H34b,H34c), C63(H63a,
 H63b,H63c), C42(H42a,H42b,H42c), C41(H41a,H41b,H41c), C65(H65a,H65b,H65c),
 C64(H64a,H64b,H64c)
;
_shelx_res_checksum              2167
_shelx_fab_checksum              68390
_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 1.626
_oxdiff_exptl_absorpt_empirical_full_min 0.589