Directing energy transfer in Pt(bodipy)(mercaptopyrene) dyads.
Irmler, Peter; Gogesch, Franciska S.; Mang, André; Bodensteiner, Michael; Larsen, Christopher B.; Wenger, Oliver S.; Winter, Rainer F.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11690–11705; doi:10.1039/c9dt01737b

data_7700356
_publ_section_title
;
 Directing energy transfer in Pt(bodipy)(mercaptopyrene) dyads.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11690
_journal_page_last               11705
_journal_paper_doi               10.1039/c9dt01737b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'2(C45 H61 B F2 N2 P2 Pt S), 1.6(C H2 Cl2), 1.4(C5 H12)'
_chemical_formula_sum            'C98.6 H142 B2 Cl3.2 F4 N4 P4 Pt2 S2'
_chemical_formula_weight         2172.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-25
_audit_creation_method
;
Olex2 1.2-alpha
(compiled Jul 26 2018 12:33:06 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-02-25 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                78.562(5)
_cell_angle_beta                 88.157(5)
_cell_angle_gamma                74.328(5)
_cell_formula_units_Z            2
_cell_length_a                   14.1734(9)
_cell_length_b                   16.7856(12)
_cell_length_c                   22.6728(15)
_cell_measurement_reflns_used    42655
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      1.73
_cell_volume                     5089.1(6)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44840
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.733
_diffrn_reflns_theta_min         1.734
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.987
_exptl_absorpt_correction_T_max  0.69316
_exptl_absorpt_correction_T_min  0.44711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'MULABS / PLATON Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13. Spek, A.L. (2009). Acta Cryst. D65, 148-155.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.640
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       0.00035(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1296
_refine_ls_number_reflns         19048
_refine_ls_number_restraints     668
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+8.2561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13599
_reflns_number_total             19048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01737b2.cif
_cod_data_source_block           pibw29
_cod_depositor_comments
'Adding full bibliography for 7700356--7700357.cif.'
_cod_original_formula_sum        'C98.60 H142 B2 Cl3.20 F4 N4 P4 Pt2 S2'
_cod_database_code               7700356
_shelx_shelxl_version_number     2018/1
_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. Restrained distances
 Pt2-S2 \\sim Pt2-S2A
 with sigma of 0.02
 S2-Pt2A \\sim S2A-Pt2A
 with sigma of 0.02
 C67-C68 \\sim C71A-C70A
 with sigma of 0.02
 C81-C68 \\sim C81A-C70A
 with sigma of 0.02
 C81-C78 \\sim C81A-C74A
 with sigma of 0.02
 C81-C74 \\sim C81A-C78A
 with sigma of 0.02
 C69-C68 \\sim C69A-C70A
 with sigma of 0.02
 S2-C67 \\sim S2A-C71A
 with sigma of 0.04
 C67-C81 \\sim C71A-C81A
 with sigma of 0.04
 C67-C69 \\sim C71A-C69A
 with sigma of 0.04
 C81-C69 \\sim C81A-C69A
 with sigma of 0.04
 C68-C78 \\sim C70A-C74A
 with sigma of 0.04
 C68-C74 \\sim C70A-C78A
 with sigma of 0.04
 C78-C74 \\sim C74A-C78A
 with sigma of 0.04
 C67-C72 \\sim C71A-C80A
 with sigma of 0.02
 C72-C73 \\sim C80A-C79A
 with sigma of 0.02
 C69-C70 \\sim C69A-C68A
 with sigma of 0.02
 C69-C80 \\sim C69A-C72A
 with sigma of 0.02
 C78-C77 \\sim C74A-C75A
 with sigma of 0.02
 C78-C79 \\sim C74A-C73A
 with sigma of 0.02
 C73-C74 \\sim C79A-C78A
 with sigma of 0.02
 C70-C71 \\sim C68A-C67A
 with sigma of 0.02
 C80-C79 \\sim C72A-C73A
 with sigma of 0.02
 C77-C76 \\sim C75A-C76A
 with sigma of 0.02
 C74-C75 \\sim C78A-C77A
 with sigma of 0.02
 C76-C75 \\sim C76A-C77A
 with sigma of 0.02
 S2-C71 \\sim S2A-C67A
 with sigma of 0.04
 C67-C73 \\sim C71A-C79A
 with sigma of 0.04
 C67-C71 \\sim C71A-C67A
 with sigma of 0.04
 C72-C68 \\sim C80A-C70A
 with sigma of 0.04
 C72-C74 \\sim C80A-C78A
 with sigma of 0.04
 C81-C73 \\sim C81A-C79A
 with sigma of 0.04
 C81-C77 \\sim C81A-C75A
 with sigma of 0.04
 C81-C79 \\sim C81A-C73A
 with sigma of 0.04
 C81-C75 \\sim C81A-C77A
 with sigma of 0.04
 C69-C71 \\sim C69A-C67A
 with sigma of 0.04
 C69-C79 \\sim C69A-C73A
 with sigma of 0.04
 C68-C70 \\sim C70A-C68A
 with sigma of 0.04
 C68-C80 \\sim C70A-C72A
 with sigma of 0.04
 C78-C80 \\sim C74A-C72A
 with sigma of 0.04
 C78-C76 \\sim C74A-C76A
 with sigma of 0.04
 C73-C75 \\sim C79A-C77A
 with sigma of 0.04
 C70-C80 \\sim C68A-C72A
 with sigma of 0.04
 C77-C79 \\sim C75A-C73A
 with sigma of 0.04
 C77-C75 \\sim C75A-C77A
 with sigma of 0.04
 C74-C76 \\sim C78A-C76A
 with sigma of 0.04
 C85A-C86A \\sim C84A-C85A \\sim C83A-C84A \\sim C83A-C82A
 with sigma of 0.005
 S2-C66 \\sim S2A-C66A
 with sigma of 0.02
 C66-C67 \\sim C66A-C71A
 with sigma of 0.02
 Pt2-C66 \\sim Pt2-C66A
 with sigma of 0.04
 C66-C68 \\sim C66A-C70A
 with sigma of 0.04
 C66-Pt2A \\sim C66A-Pt2A
 with sigma of 0.04
 C66-C71 \\sim C66A-C67A
 with sigma of 0.02
 C66-C72 \\sim C66A-C80A
 with sigma of 0.04
 C66-C70 \\sim C66A-C68A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C82A \\sim Cl2 \\sim C100 \\sim C83A \\sim C84A \\sim Cl1 \\sim C85A \\sim
C86A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C67 \\sim C72 \\sim C81 \\sim C69 \\sim C68 \\sim C78 \\sim C73 \\sim C70 \\sim
C71 \\sim C80 \\sim C77 \\sim C74 \\sim C76 \\sim C79 \\sim C75 \\sim C67A
\\sim C68A \\sim C69A \\sim C71A \\sim C70A \\sim C80A \\sim C79A \\sim C78A
\\sim C77A \\sim C76A \\sim C75A \\sim C74A \\sim C81A \\sim C72A \\sim C73A:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(Pt2) = Uanis(Pt2A)
Uanis(C66) = Uanis(C66A)
4. Others
 Sof(Pt2A)=Sof(S2A)=Sof(C66A)=Sof(C67A)=Sof(H67A)=Sof(C68A)=Sof(H68A)=
 Sof(C69A)=Sof(C71A)=Sof(C70A)=Sof(C80A)=Sof(H80A)=Sof(C79A)=Sof(H79A)=
 Sof(C78A)=Sof(C77A)=Sof(H77A)=Sof(C76A)=Sof(H76A)=Sof(C75A)=Sof(H75A)=
 Sof(C74A)=Sof(C81A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73A)=1-FVAR(1)
 Sof(Pt2)=Sof(S2)=Sof(C66)=Sof(C67)=Sof(C72)=Sof(H72)=Sof(C81)=Sof(C69)=
 Sof(C68)=Sof(C78)=Sof(C73)=Sof(H73)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(H71)=
 Sof(C80)=Sof(H80)=Sof(C77)=Sof(H77)=Sof(C74)=Sof(C76)=Sof(H76)=Sof(C79)=
 Sof(H79)=Sof(C75)=Sof(H75)=FVAR(1)
 Fixed Sof: Cl1(0.6) Cl2(0.6) C100(0.6) H10C(0.6) H10D(0.6) C86A(0.4)
 H86D(0.4) H86E(0.4) H86F(0.4) C84A(0.4) H84D(0.4) H84E(0.4) C85A(0.4)
 H85C(0.4) H85D(0.4) C83A(0.4) H83C(0.4) H83D(0.4) C82A(0.4) H82A(0.4)
 H82B(0.4) H82C(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C83(H83A,H83B), C16(H16A,H16B), C89(H89A,H89B), C87(H87A,
 H87B), C42(H42A,H42B), C93(H93A,H93B), C40(H40A,H40B), C85(H85A,H85B),
 C59(H59A,H59B), C45(H45A,H45B), C38(H38A,H38B), C36(H36A,H36B), C91(H91A,H91B),
  C63(H63A,H63B), C12(H12A,H12B), C97(H97A,H97B), C96(H96A,H96B), C98(H98A,
 H98B), C101(H10A,H10B), C100(H10C,H10D), C84A(H84D,H84E), C85A(H85C,H85D),
 C83A(H83C,H83D)
5.b Me refined with riding coordinates:
 C58(H58A,H58B,H58C)
5.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C72(H72), C30(H30), C32(H32), C21(H21), C25(H25), C73(H73),
 C70(H70), C71(H71), C33(H33), C80(H80), C26(H26), C77(H77), C28(H28), C76(H76),
  C79(H79), C29(H29), C75(H75), C67A(H67A), C68A(H68A), C80A(H80A), C79A(H79A),
 C77A(H77A), C76A(H76A), C75A(H75A), C72A(H72A), C73A(H73A)
5.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C86(H86A,H86B,H86C), C65(H65A,H65B,H65C), C39(H39A,H39B,
 H39C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C61(H61A,H61B,H61C), C43(H43A,
 H43B,H43C), C48(H48A,H48B,H48C), C84(H84A,H84B,H84C), C37(H37A,H37B,H37C),
 C88(H88A,H88B,H88C), C94(H94A,H94B,H94C), C62(H62A,H62B,H62C), C41(H41A,H41B,
 H41C), C90(H90A,H90B,H90C), C60(H60A,H60B,H60C), C17(H17A,H17B,H17C), C46(H46A,
 H46B,H46C), C92(H92A,H92B,H92C), C64(H64A,H64B,H64C), C14(H14A,H14B,H14C),
 C13(H13A,H13B,H13C), C95(H95A,H95B,H95C), C99(H99A,H99B,H99C), C86A(H86D,H86E,
 H86F), C82A(H82A,H82B,H82C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88260
_olex2_submission_special_instructions 'No special instructions were received'