Extended tetrathiafulvalene with a pentaleno[1,2-<i>b</i>:4,5-<i>b</i>']difluorene core - a donor-acceptor multi-redox system.
Granhøj, Jeppe; Pedersen, Viktor Bliksted Roug; Mikkelsen, Kurt V.; Nielsen, Mogens Brøndsted; Organic & biomolecular chemistry 22 (2024) 9259–9265; doi:10.1039/d4ob01755b

data_7160236
_publ_section_title
;
 Extended tetrathiafulvalene with a
 pentaleno[1,2-<i>b</i>:4,5-<i>b</i>']difluorene core - a donor-acceptor
 multi-redox system.
;
_journal_issue                   47
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9259
_journal_page_last               9265
_journal_paper_doi               10.1039/d4ob01755b
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C48 H34 O2, C H2 Cl2  '
_chemical_formula_sum            'C49 H36 Cl2 O2'
_chemical_formula_weight         727.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V143 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2024-10-03 deposited with the CCDC.	2024-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                87.358(4)
_cell_angle_beta                 77.624(6)
_cell_angle_gamma                87.173(5)
_cell_formula_units_Z            1
_cell_length_a                   8.0184(9)
_cell_length_b                   9.0834(7)
_cell_length_c                   12.9502(12)
_cell_measurement_reflns_used    3915
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7475
_cell_measurement_theta_min      2.6025
_cell_volume                     919.57(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       APEX4
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39614
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.246
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_recrystallization_method
'Single crystals were obtained from diffusion of methanol into a solution of the compound in dichloromethane from a bilayer system.'
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3757
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0489P)^2^+0.4923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2787
_reflns_number_total             3757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01755b2.cif
_cod_data_source_block           mo_D8V6035_0m_a
_cod_depositor_comments
'Adding full bibliography for 7160236--7160237.cif.'
_cod_database_code               7160236
_shelx_shelxl_version_number     2019/2
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              5737