New π-extended catecholato complexes of Pt(ii) and Pd(ii) containing a benzothienobenzothiophene (BTBT) moiety: synthesis, electrochemical behavior and charge transfer properties.
Tahara, Keishiro; Ashihara, Yuya; Higashino, Toshiki; Ozawa, Yoshiki; Kadoya, Tomofumi; Sugimoto, Kunihisa; Ueda, Akira; Mori, Hatsumi; Abe, Masaaki; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7367–7377; doi:10.1039/c8dt05057k

data_7049601
_publ_section_title
;
 New \p-extended catecholato complexes of Pt(ii) and Pd(ii) containing a
 benzothienobenzothiophene (BTBT) moiety: synthesis, electrochemical
 behavior and charge transfer properties.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7367
_journal_page_last               7377
_journal_paper_doi               10.1039/c8dt05057k
_journal_volume                  48
_journal_year                    2019
_chemical_compound_source        'synthesis as described'
_chemical_formula_sum            'C33 H31.5 N2.5 O2 Pd S2'
_chemical_formula_weight         665.63
_chemical_name_common            PdBTBT
_chemical_name_systematic        PdBTBT
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2018-12-05T17:04:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-12-17 deposited with the CCDC.    2019-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.918(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.413(3)
_cell_length_b                   17.240(5)
_cell_length_c                   14.457(4)
_cell_measurement_reflns_used    12547
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.33
_cell_measurement_theta_min      0.5
_cell_measurement_wavelength     0.3009
_cell_volume                     2908.7(14)
_computing_cell_refinement       'R-AXIS (Rigaku Co. Ltd., 2008)'
_computing_data_collection       'R-AXIS (Rigaku Co. Ltd., 2008)'
_computing_data_reduction
'RAPID-AUTO (Rigaku, 2008), SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'quarter \C-circle diffractometer'
_diffrn_measurement_device_type
'SPring-8 BL02B1 Dectris PILATUS3 X 1M CdTe HPC detector'
_diffrn_measurement_method       '\w axis oscillation'
_diffrn_orient_matrix_UB_11      -0.02277
_diffrn_orient_matrix_UB_12      0.055672
_diffrn_orient_matrix_UB_13      -0.000393
_diffrn_orient_matrix_UB_21      0.081558
_diffrn_orient_matrix_UB_22      0.014283
_diffrn_orient_matrix_UB_23      0.036512
_diffrn_orient_matrix_UB_31      0.013136
_diffrn_orient_matrix_UB_32      0.007823
_diffrn_orient_matrix_UB_33      -0.063871
_diffrn_radiation_monochromator  'Si 311'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3009
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43288
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        10.401
_diffrn_reflns_theta_max         11.267
_diffrn_reflns_theta_min         0.793
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.4
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.52
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6670
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0
_reflns_number_gt                5270
_reflns_number_total             6670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05057k2.cif
_cod_data_source_block           pdBTBT
_cod_depositor_comments          'Adding full bibliography for 7049601.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C33 H31.50 N2.50 O2 Pd S2'
_cod_database_code               7049601
_shelx_estimated_absorpt_t_min   0.98
_shelx_estimated_absorpt_t_max   0.992