Planar Benzo[1,2- b:4,5- b']dithiophene Derivatives Decorated with Nitronyl and Imino Nitroxides.
Kolanji, Kubandiran; Postulka, Lars; Wolf, Bernd; Lang, Michael; Schollmeyer, Dieter; Baumgarten, Martin; The Journal of organic chemistry 84 (2019) 140–149; doi:10.1021/acs.joc.8b02499

data_4035922
_publ_section_title
;
 Planar Benzo[1,2- b:4,5- b']dithiophene Derivatives Decorated with
 Nitronyl and Imino Nitroxides.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              140
_journal_page_last               149
_journal_paper_doi               10.1021/acs.joc.8b02499
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C58 H98 N4 O6 S4 Si4'
_chemical_formula_sum            'C58 H98 N4 O6 S4 Si4'
_chemical_formula_weight         1188.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.054(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   48.0321(15)
_cell_length_b                   10.6191(2)
_cell_length_c                   14.3112(5)
_cell_measurement_reflns_used    17282
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.31
_cell_volume                     7227.5(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT - 2014'
_diffrn_ambient_temperature      193(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 152 frames, detector distance = 80 mm'
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22829
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.446
_diffrn_reflns_theta_min         2.308
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_T_max  0.9739
_exptl_absorpt_correction_T_min  0.8354
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       needle
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.740
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
TITL tbdttnnsi in C2/c Ohne LSgm
CELL   48.0321   10.6191   14.3112     90.00     98.05     90.00
SPGR C2/c
C101 1.000 0.336 0.365 !      11.04 eA-3
C102 0.992 0.273 0.242 !       2.82 eA-3
Q103 0.973 0.091 0.468 !       0.64 eA-3
Q104 0.519 0.403 0.491 !       0.61 eA-3
Q105 0.528 0.343 0.356 !       0.55 eA-3
Q106 0.809 0.126 0.105 !       0.55 eA-3
Q107 0.196 0.059 0.190 !       0.54 eA-3
Q108 0.493 0.503 0.398 !       0.53 eA-3
Q109 0.182 0.504 0.950 !       0.53 eA-3
Q110 0.207 0.163 0.958 !       0.52 eA-3
Q111 0.496 0.453 0.081 !       0.51 eA-3
;
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6185
_reflns_number_total             9067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b02499_si_002.cif
_cod_data_source_block           bdtth2-nnsi
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4035922
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              710
_shelx_hkl_checksum              65700
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              27469