The semiquinone radical anion of 1,10-phenanthroline-5,6-dione: synthesis and rare earth coordination chemistry.
Hickson, James R.; Horsewill, Samuel J.; McGuire, Jake; Wilson, Claire; Sproules, Stephen; Farnaby, Joy H.; Chemical communications (Cambridge, England) 54 (2018) 11284–11287; doi:10.1039/c8cc05591b

data_7122354
_publ_section_title
;
 The semiquinone radical anion of 1,10-phenanthroline-5,6-dione: synthesis
 and rare earth coordination chemistry.
;
_journal_issue                   80
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11284
_journal_page_last               11287
_journal_paper_doi               10.1039/c8cc05591b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C10 H10 Co, C12 H6 N2 O2'
_chemical_formula_sum            'C22 H16 Co N2 O2'
_chemical_formula_weight         399.30
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-06 deposited with the CCDC.
2018-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.199(2)
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   40.770(2)
_cell_length_b                   8.4491(4)
_cell_length_c                   43.181(2)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.73
_cell_volume                     13959.8(12)
_computing_cell_refinement       'SAINT V8.37A (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'APEX3 Ver. 2016.9-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            76973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_min         2.370
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1239 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.8676. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       shard
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         17302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0591P)^2^+11.6597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12054
_reflns_number_total             17302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05591b2.cif
_cod_data_source_block           CoCp2pd
_cod_depositor_comments
'Adding full bibliography for 7122354--7122355.cif.'
_cod_original_cell_volume        13959.7(13)
_cod_database_code               7122354
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.832
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C101(H101), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C121(H121), C122(H122), C123(H123), C124(H124),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129), C130(H130),
 C131(H131), C132(H132), C133(H133), C134(H134), C135(H135), C136(H136),
 C137(H137), C138(H138), C139(H139), C140(H140), C1(H1), C2(H2), C3(H3), C8(H8),
  C9(H9), C10(H10), C1A(H1A), C2A(H2A), C3A(H3A), C8A(H8A), C9A(H9A),
 C10A(H10A), C1B(H1B), C2B(H2B), C3B(H3B), C8B(H8B), C9B(H9B), C10B(H10B),
 C1C(H1C), C2C(H2C), C3C(H3C), C8C(H8C), C9C(H9C), C10C(H10C)
;
_shelx_res_checksum              45501
_olex2_submission_special_instructions 'No special instructions were received'