Selective reduction of 1,5-diazacyclooctatetraenes: synthesis and structures of aromatic diazacyclooctatetraenyl dianions and 2,6-bipyrrolinyl dianionic Co(II) complex
Huang, Zhe; Tan, Genwen; Chen, Chao; Zhang, Wen-Xiong; Wang, Xinping; Xi, Zhenfeng; Chemical Communications  (2019) –; doi:10.1039/C9CC00075E

data_7122939
_publ_section_title
;
 Selective reduction of 1,5-diazacyclooctatetraenes: synthesis and
 structures of aromatic diazacyclooctatetraenyl dianions and
 2,6-bipyrrolinyl dianionic Co(II) complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00075E
_journal_year                    2019
_chemical_formula_sum            'C84 H112 Co2 N6'
_chemical_formula_weight         1323.65
_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
_audit_update_record
;
2018-12-03 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.497(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3208(18)
_cell_length_b                   14.4351(12)
_cell_length_c                   25.484(2)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.23
_cell_volume                     8505.5(12)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            56408
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.142
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2016/2 (Bruker AXS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         14951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0552P)^2^+4.4647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12054
_reflns_number_total             14951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00075e2.cif
_cod_data_source_block           p21n_a_sq
_cod_original_cell_volume        8505.4(12)
_cod_database_code               7122939
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              81692
_shelx_fab_checksum              27729