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_1556901
_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, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C67 H79 B2 F8 N7 O6 Pt'
_chemical_formula_weight         1447.08
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-10-31
_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                105.665(4)
_cell_angle_beta                 99.693(4)
_cell_angle_gamma                96.105(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1982(5)
_cell_length_b                   18.2063(7)
_cell_length_c                   19.7708(8)
_cell_measurement_reflns_used    9702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.7220
_cell_measurement_theta_min      1.8030
_cell_volume                     3439.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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
;
Superflip n/a (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -106.00  20.00   1.00   60.00    --  -16.70 -60.00-120.00  126
  2  \w   -106.00  20.00   1.00   60.00    --  -16.70 -60.00  30.00  126
  3  \w   -106.00  20.00   1.00   60.00    --  -16.70 -60.00-180.00  126
  4  \w   -106.00  20.00   1.00   60.00    --  -16.70 -60.00 -60.00  126
  5  \w   -106.00  20.00   1.00   60.00    --  -16.70 -60.00 150.00  126
  6  \w   -106.00  20.00   1.00   60.00    --  -16.70 -60.00 -30.00  126
  7  \w   -106.00  19.00   1.00   60.00    --  -16.70 -57.00  90.00  125
  8  \w    -53.00  37.00   1.00   60.00    --  -16.70  60.00-120.00   90
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ 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      -0.0212551000
_diffrn_orient_matrix_UB_12      -0.0397251000
_diffrn_orient_matrix_UB_13      -0.0188968000
_diffrn_orient_matrix_UB_21      -0.0428441000
_diffrn_orient_matrix_UB_22      -0.0031408000
_diffrn_orient_matrix_UB_23      0.0242071000
_diffrn_orient_matrix_UB_31      -0.0531192000
_diffrn_orient_matrix_UB_32      0.0096050000
_diffrn_orient_matrix_UB_33      -0.0225099000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1614
_diffrn_reflns_av_unetI/netI     0.1418
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54267
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         1.826
_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    2.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (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    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.796
_refine_diff_density_min         -1.885
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         12157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0732
_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^)+(0.0820P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7976
_reflns_number_total             12157
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05507j2.cif
_cod_data_source_block           zzix-23_k
_cod_depositor_comments
;Adding full bibliography for 1556900--1556906.cif.

 Adding full bibliography for 1556900--1556906.cif.
;
_cod_database_code               1556901
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C65H76B2F8N6O6Pt
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.902
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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, All C(H,H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C68(H68A,H68B), C81(H81A,H81B), C83(H83A,H83B), C86(H86A,
 H86B), C92(H92A,H92B), C95(H95A,H95B), C100(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C45(H45), C5(H5), C9(H9), C14(H14A), C25(H25), C29(H29), C32(H32),
 C37(H37), C39(H39), C41(H41), C44(H44), C2(H2), C8(H8), C13(H13), C24(H24),
 C30(H30), C27(H27), C43(H43), C54(H54), C62(H62), C66(H66), C79(H79)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C35(H35A,H35B,
 H35C), C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C47(H47A,H47B,H47C), C70(H70A,
 H70B,H70C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C76(H76A,H76B,H76C),
 C87(H87A,H87B,H87C), C10(H10C,H10D,H10E)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69446
_shelx_fab_checksum              65163
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 11.828
_oxdiff_exptl_absorpt_empirical_full_min 0.279