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_4032638
_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         'C25 H47 Br N2 O2 Si2'
_chemical_formula_sum            'C25 H47 Br N2 O2 Si2'
_chemical_formula_weight         543.73
_chemical_name_systematic
;
2-(4-bromophenyl)-1,3-bis((tert-butyldimethylsilyl)oxy)-4,4,5,5-
tetramethylimidazolidine
;
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                92.856(4)
_cell_angle_beta                 94.940(4)
_cell_angle_gamma                103.966(4)
_cell_formula_units_Z            2
_cell_length_a                   7.1928(3)
_cell_length_b                   11.2760(5)
_cell_length_c                   19.2222(9)
_cell_measurement_reflns_used    18628
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.22
_cell_volume                     1503.30(12)
_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      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 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      ' 228 frames, detector distance = 70 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  0.0205
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14704
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.156
_diffrn_reflns_theta_min         2.216
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.469
_exptl_absorpt_correction_T_max  0.7908
_exptl_absorpt_correction_T_min  0.5697
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         7340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0343P)^2^+0.7192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5915
_reflns_number_total             7340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00435_si_002.cif
_cod_data_source_block           5
_cod_database_code               4032638
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.539
_shelx_estimated_absorpt_t_max   0.758
_shelx_res_checksum              87602
_shelx_hkl_checksum              48828