Mixed Phenyl and Thiophene Oligomers for Bridging Nitronyl Nitroxides.
Kolanji, Kubandiran; Ravat, Prince; Bogomyakov, Artem S.; Ovcharenko, Victor I.; Schollmeyer, Dieter; Baumgarten, Martin; The Journal of organic chemistry  (2017) –; doi:10.1021/acs.joc.7b00435

data_4032636
_publ_section_title
;
 Mixed Phenyl and Thiophene Oligomers for Bridging Nitronyl Nitroxides.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.7b00435
_journal_year                    2017
_chemical_formula_moiety         'C32 H36 N4 O4'
_chemical_formula_sum            'C32 H36 N4 O4'
_chemical_formula_weight         540.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 112.061(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5064(9)
_cell_length_b                   9.9143(10)
_cell_length_c                   12.9226(12)
_cell_measurement_reflns_used    12972
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      64.46
_cell_measurement_theta_min      4.40
_cell_volume                     1366.3(2)
_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    SIR-2004
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      ' 924 frames, detector distance = 40 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'X-ray mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11670
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.849
_diffrn_reflns_theta_min         4.395
_diffrn_source                   'Incoatec microSource Cu'
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_correction_T_min  0.9620
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.049(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1587
_refine_ls_R_factor_gt           0.0963
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.2959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1230
_reflns_number_total             2446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00435_si_002.cif
_cod_data_source_block           pppnn
_cod_original_cell_volume        1366.2(2)
_cod_database_code               4032636
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              48581
_shelx_hkl_checksum              2852