Triplet state CPL active helicene-dithiolene platinum bipyridine complexes
Biet, Thomas; Cauchy, Thomas; Sun, Qinchao; Ding, Jie; Hauser, Andreas; Oulevey, Patric; Bürgi, Thomas; Jacquemin, Denis; Vanthuyne, Nicolas; Crassous, Jeanne; Avarvari, Narcis; Chem. Commun.  (2017) –; doi:10.1039/C7CC05198K

data_7120497
_publ_section_title
;
 Triplet state CPL active helicene-dithiolene platinum bipyridine
 complexes
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05198K
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H22 N2 Pt S2, C6 H12'
_chemical_formula_sum            'C42 H44 N2 Pt S2'
_chemical_formula_weight         825.92
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-19T17:06:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-05-15 deposited with the CCDC.
2017-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   21.1835(3)
_cell_length_b                   21.2582(3)
_cell_length_c                   27.7753(4)
_cell_measurement_reflns_used    16042
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      76.155
_cell_measurement_theta_min      2.588
_cell_volume                     12507.9(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, V1.171.37.35g'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, V1.171.37.35g'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, V1.171.37.35g'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 5.199
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            45888
_diffrn_reflns_theta_full        76.55
_diffrn_reflns_theta_max         76.55
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    9.912
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.6506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
        (compiled Dec  9 2014,15:38:47)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.2292
_exptl_crystal_size_mid          0.0327
_exptl_crystal_size_min          0.0306
_platon_squeeze_details
;
The unit cell contains disordered cyclohexane molecules which were not modelled
but the corresponding density was taken into account using SQUEEZE/PLATON
procedure. The unit cell contains 12 holes with disordered solvent and each hole
of contains about 47 or 91 electrons which corresponds to 1 or 2 cyclohexane 
molecules per hole. The new composition (16 cyclohexane molecules per unit cell) was included in the calculation of the empirical formula, formula weight,
density, linear absorption coefficient and F(000).
;
_refine_diff_density_max         1.82
_refine_diff_density_min         -1.416
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1477
_refine_ls_number_reflns         23584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+9.4517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                19856
_reflns_number_total             23584
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;

2017-11-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C168 H136 N8 Pt4 S8'
_cod_original_formula_weight         3303.69
_cod_original_formula_moiety         '4(C36 H22 N2 Pt S2), 4(C6 H12)'
_cod_original_formula_units_Z            4
_cod_data_source_file            c7cc05198k2.cif
_cod_data_source_block           squeezed
_cod_database_code               7120497