A novel Pt(iv) mono azido mono triazolato complex evolves azidyl radicals following irradiation with visible light.
Yao, Kezi; Bertran, Arnau; Morgan, Jacques; Hare, Samuel M.; Rees, Nicholas H.; Kenwright, Alan M.; Edkins, Katharina; Bowen, Alice M.; Farrer, Nicola J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6416–6420; doi:10.1039/c9dt01156k

data_7049800
_publ_section_title
;
 A novel Pt(iv) mono azido mono triazolato complex evolves azidyl radicals
 following irradiation with visible light.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6416
_journal_page_last               6420
_journal_paper_doi               10.1039/c9dt01156k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C26 H22 N8 O4 Pt, C5 H10 O'
_chemical_formula_sum            'C31 H32 N8 O5 Pt'
_chemical_formula_weight         791.73
_chemical_name_systematic        'complex 3b'
_chemical_properties_physical    Light-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-12-07 deposited with the CCDC.    2019-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5699(6)
_cell_length_b                   13.6495(5)
_cell_length_c                   28.6384(12)
_cell_measurement_reflns_used    6671
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.9780
_cell_measurement_theta_min      4.1210
_cell_volume                     6086.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0509
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.844
_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  87.00   1.00    4.24    --   14.84 178.00  60.00   52
  2  \w     35.00  70.00   1.00    4.24    --   14.84 178.00-180.00   35
  3  \w    -41.00  37.00   1.00    4.24    --   14.84 -77.00-120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0036674000
_diffrn_orient_matrix_UB_12      0.0244838000
_diffrn_orient_matrix_UB_13      -0.0217939000
_diffrn_orient_matrix_UB_21      -0.0441012000
_diffrn_orient_matrix_UB_22      -0.0092594000
_diffrn_orient_matrix_UB_23      -0.0044823000
_diffrn_orient_matrix_UB_31      -0.0109522000
_diffrn_orient_matrix_UB_32      0.0448290000
_diffrn_orient_matrix_UB_33      0.0109040000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20849
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.196
_diffrn_reflns_theta_min         3.470
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.666
_exptl_absorpt_correction_T_max  0.504
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.728
_exptl_crystal_description       prism
_exptl_crystal_F_000             3136
_exptl_crystal_preparation       'Cut from a larger crystal'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN/tetrahydropyran'
_exptl_crystal_size_max          0.651
_exptl_crystal_size_mid          0.321
_exptl_crystal_size_min          0.155
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.797
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         6965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0062P)^2^+24.6767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5767
_reflns_number_total             6965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01156k2.cif
_cod_data_source_block           18ke08
_cod_depositor_comments          'Adding full bibliography for 7049800.cif.'
_cod_database_code               7049800
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C31 H33 N8 O5 Pt'
_reflns_odcompleteness_completeness 99.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 O(H) groups
2.a Rotating group:
 O6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C41(H41A,H41B), C45(H45A,H45B), C42(H42A,H42B), C1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C27(H27), C25(H25), C23(H23), C24(H24), C21(H21), C22(H22),
 C28(H28), C32(H32), C40(H40), C33(H33), C39(H39), C34(H34), C37(H37), C36(H36),
  C29(H29), C35(H35), C30(H30), C38(H38), C31(H31)
2.d Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_olex2_date_sample_data_collection 2018-05-23
_olex2_exptl_crystal_mounting_method
'Crystal soaked in perfluoro polyether oil and mounted on a MiTeGen loop directly into the pre-cooled cryostream'
_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 1.392
_oxdiff_exptl_absorpt_empirical_full_min 0.687