Isolation of a Stable Pyridine Radical Anion
Schröder, Jan; Himmel, Daniel; Kratzert, Daniel; Radtke, Valentin; Richert, Sabine; Weber, Stefan; Böttcher, Tobias; Chemical Communications  (2019) –; doi:10.1039/C8CC09700C

data_7122784
_publ_section_title
;
 Isolation of a Stable Pyridine Radical Anion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09700C
_journal_year                    2019
_chemical_formula_sum            'C21 H39 B2 K N5'
_chemical_formula_weight         422.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-11-20 deposited with the CCDC.
2019-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.951(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   5.7782(4)
_cell_length_c                   17.2288(11)
_cell_measurement_reflns_used    6023
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      49.975
_cell_measurement_theta_min      4.729
_cell_volume                     2409.0(3)
_computing_cell_refinement       'SAINT V8.37A'
_computing_data_collection       'APEX3 v2016.9-0'
_computing_data_reduction        'SAINT V8.37A'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33738
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.893
_diffrn_reflns_theta_min         0.841
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       needle
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.150
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_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5730
_refine_ls_number_restraints     411
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0638P)^2^+0.8418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1511
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4078
_reflns_number_total             5730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09700c2.cif
_cod_data_source_block           p21c_a
_cod_database_code               7122784
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              11093