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_7122355
_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 H7 N2 O2)'
_chemical_formula_sum            'C22 H17 Co N2 O2'
_chemical_formula_weight         400.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-07-06 deposited with the CCDC.
2018-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.4592(4)
_cell_length_b                   18.0502(7)
_cell_length_c                   20.2671(8)
_cell_measurement_reflns_used    6492
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.4100
_cell_measurement_theta_min      3.2510
_cell_volume                     3460.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -79.00 -53.00   0.50    5.00    --    5.00  57.00-164.00   52
  2  \w    -89.00  78.00   0.50    5.00    --    0.00  60.00-120.00  334
  3  \w   -133.00 -93.00   0.50   35.00    --  -90.00  60.00 120.00   80
  4  \w    -66.00 -29.00   0.50   35.00    --  -90.00  60.00 120.00   74
  5  \w   -179.00-139.00   0.50   35.00    --  -90.00  60.00 120.00   80
  6  \w   -178.00-152.00   0.50   35.00    --  -90.00  60.00-120.00   52
  7  \w   -127.00 -93.00   0.50   35.00    --  -90.00  60.00-120.00   68
  8  \w    -67.00 -41.00   0.50   35.00    --  -90.00  60.00-120.00   52
  9  \w   -179.00  -1.00   0.50   35.00    --  -90.00  57.00-164.00  356
 10  \w   -125.00 -99.00   0.50   35.00    --  -90.00  43.00 120.00   52
 11  \w    -76.00 -50.00   0.50   35.00    --  -90.00  43.00 120.00   52
 12  \w    -97.00  -1.00   0.50   35.00    --  -90.00  29.00  60.00  192
 13  \w   -143.00-117.00   0.50   35.00    --  -90.00  29.00 -90.00   52
 14  \w    -73.00  -1.00   0.50   35.00    --  -90.00  29.00 -90.00  144
 15  \w   -178.00-120.00   0.50   35.00    --  -90.00  29.00  60.00  116
 16  \w   -122.00  -9.00   0.50   35.00    --  -90.00  29.00 -60.00  226
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0717953000
_diffrn_orient_matrix_UB_12      0.0192420000
_diffrn_orient_matrix_UB_13      -0.0660712000
_diffrn_orient_matrix_UB_21      -0.0667451000
_diffrn_orient_matrix_UB_22      -0.0690002000
_diffrn_orient_matrix_UB_23      -0.0318775000
_diffrn_orient_matrix_UB_31      -0.1299095000
_diffrn_orient_matrix_UB_32      0.0464509000
_diffrn_orient_matrix_UB_33      -0.0200325000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25906
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.279
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    7.940
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       'opaque blade'
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 1506 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.036(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         6301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0858P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                4652
_reflns_number_total             6301
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05591b2.cif
_cod_data_source_block           CpCp2C12H7N2O2
_cod_depositor_comments
'Adding full bibliography for 7122354--7122355.cif.'
_cod_database_code               7122355
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C22 H16 N2 O2 Co'
_chemical_oxdiff_usercomment     JHGLA170
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.606
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1C(H1C), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C6C(H6C), C7C(H7C),
 C8C(H8C), C9C(H9C), C10C(H10C), C11C(H11C), C12C(H12C), C13C(H13C), C14C(H14C),
  C15C(H15C), C16C(H16C), C17C(H17C), C18C(H18C), C19C(H19C), C20C(H20C),
 C1(H1A), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C1A(H1AA), C2A(H2AA),
 C3A(H3A), C8A(H8A), C9A(H9A), C10A(H10A)
;
_shelx_res_checksum              16427
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.631
_oxdiff_exptl_absorpt_empirical_full_min 0.549