Synthesis, Spectroscopic Properties, and Photoconductivity of Black Absorbers Consisting of Pt(Bipyridine)(Dithiolate) Charge Transfer Complexes in the Presence and Absence of Nitrofluorenone Acceptors.
Browning, Charles; Hudson, Joshua M.; Reinheimer, Eric W.; Kuo, Fang-Ling; McDougald, Jr, Roy N; Rabaâ, Hassan; Pan, Hongjun; Bacsa, John; Wang, Xiaoping; Dunbar, Kim R.; Shepherd, Nigel D.; Omary, Mohammad A.; Journal of the American Chemical Society  (2014) 141107065104007–; doi:10.1021/ja506583k

data_4122895
_publ_section_title
;
 Synthesis, Spectroscopic Properties, and Photoconductivity of Black
 Absorbers Consisting of Pt(Bipyridine)(Dithiolate) Charge Transfer
 Complexes in the Presence and Absence of Nitrofluorenone Acceptors.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141107065104007
_journal_paper_doi               10.1021/ja506583k
_journal_year                    2014
_chemical_formula_moiety         'C25 H30 N2 Pt S2, C13 H6 N2 O5, C3 H3'
_chemical_formula_sum            'C41 H39 N4 O5 Pt S2'
_chemical_formula_weight         926.97
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                75.51(3)
_cell_angle_beta                 86.77(3)
_cell_angle_gamma                69.05(3)
_cell_formula_units_Z            2
_cell_length_a                   11.298(2)
_cell_length_b                   13.599(3)
_cell_length_c                   13.964(3)
_cell_measurement_reflns_used    4717
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.750
_cell_measurement_theta_min      2.406
_cell_volume                     1938.6(8)
_computing_cell_refinement       'SAINT V6.34B (Bruker, 2006)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT V6.34B (Bruker, 2006)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24368
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.601
_diffrn_reflns_theta_min         1.507
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.776
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0869 before and 0.0494 after correction.
The Ratio of minimum to maximum transmission is 0.7953.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       prism
_exptl_crystal_F_000             926
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by slow evaporation'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.988
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8504
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7303
_reflns_number_total             8504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja506583k_si_001.cif
_cod_data_source_block           compound1
_cod_database_code               4122895
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C4 \\sim C7'-C5
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, C6, C5, C4, C7, C3, C2, C7'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, C30, C31, C32, N4, O4, O5, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H4)=Sof(C7')=Sof(H7'A)=Sof(H7'B)=Sof(H7'C)=1-FVAR(1)
 Sof(H5)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C11(H11), C18(H18), C21(H21), C3(H3), C20(H20), C10(H10), C4(H4),
 C6(H6), C5(H5), C27(H27), C38(H38), C34(H34), C37(H37), C31(H31), C33(H33),
 C39(H39), C40(H40), C41(H41)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C7'(H7'A,
 H7'B,H7'C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id ER012
_olex2_submission_special_instructions 'No special instructions were received'