Analysis of Lanthanide-Radical Magnetic Interactions in Ce(III) 2,2'-Bipyridyl Complexes.
Ortu, Fabrizio; Liu, Jingjing; Burton, Matthew; Fowler, Jonathan M.; Formanuik, Alasdair; Boulon, Marie-Emmanuelle; Chilton, Nicholas F.; Mills, David P.; Inorganic chemistry 56 (2017) 2496–2505; doi:10.1021/acs.inorgchem.6b02683

data_4349356
_publ_section_title
;
 Analysis of Lanthanide-Radical Magnetic Interactions in Ce(III)
 2,2'-Bipyridyl Complexes.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2496
_journal_page_last               2505
_journal_paper_doi               10.1021/acs.inorgchem.6b02683
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C38 H66 Ce N2 Si6'
_chemical_formula_sum            'C38 H66 Ce N2 Si6'
_chemical_formula_weight         859.58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.9857(14)
_cell_length_b                   18.2507(17)
_cell_length_c                   28.791(3)
_cell_measurement_reflns_used    2225
_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      22.7690
_cell_measurement_theta_min      3.5910
_cell_volume                     9450.7(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   28.00   54.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   60.0000 26

  2 omega   35.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  178.0000  -90.0000 59

  3 omega   46.00   81.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601   37.0000   90.0000 35

  4 omega   36.00   95.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  178.0000   30.0000 59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0234453000
_diffrn_orient_matrix_UB_12      -0.0275998000
_diffrn_orient_matrix_UB_13      -0.0092731000
_diffrn_orient_matrix_UB_21      -0.0311654000
_diffrn_orient_matrix_UB_22      0.0234422000
_diffrn_orient_matrix_UB_23      0.0027385000
_diffrn_orient_matrix_UB_31      0.0058494000
_diffrn_orient_matrix_UB_32      0.0141471000
_diffrn_orient_matrix_UB_33      -0.0226515000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1158
_diffrn_reflns_av_unetI/netI     0.1665
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            28201
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.349
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.246
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.1703
_exptl_crystal_size_mid          0.0753
_exptl_crystal_size_min          0.0493
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8619
_refine_ls_number_restraints     282
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.0674
_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^)+(0.0191P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3978
_reflns_number_total             8619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02683_si_002.cif
_cod_data_source_block           4
_cod_database_code               4349356
_manchester_internal_coll_name   adpm145
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 25s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   05/03/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 07/03/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 07/03/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 07/03/2015
_manchester_internal_validation_user FO
_manchester_internal_validation_date 24/11/2015
_manchester_internal_archive_date 24/11/2015
_chemical_oxdiff_formula         'C40 Si6 Ce N2'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.004 and sigma
for terminal atoms of 0.008
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C29(H29), C30(H30), C31(H31), C32(H32),
 C35(H35), C36(H36), C37(H37), C38(H38)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              18211
_shelx_hkl_checksum              82435
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'