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_4349353
_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         'C36 H50 La N2'
_chemical_formula_sum            'C36 H50 La N2'
_chemical_formula_weight         649.69
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.307(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6336(13)
_cell_length_b                   10.6734(6)
_cell_length_c                   19.3376(9)
_cell_measurement_reflns_used    2609
_cell_measurement_temperature    150.03(10)
_cell_measurement_theta_max      26.2680
_cell_measurement_theta_min      3.6680
_cell_volume                     3341.0(4)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.03(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -5.00   26.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -99.0000   60.0000 31

  2 omega  -18.00   26.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -99.0000  -60.0000 44

  3 omega    0.00   89.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0662   57.0000   90.0000 89

  4 omega  -17.00   73.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0662   37.0000   30.0000 90
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0433573000
_diffrn_orient_matrix_UB_12      -0.0089345000
_diffrn_orient_matrix_UB_13      0.0107168000
_diffrn_orient_matrix_UB_21      0.0016950000
_diffrn_orient_matrix_UB_22      -0.0098638000
_diffrn_orient_matrix_UB_23      -0.0359107000
_diffrn_orient_matrix_UB_31      0.0060935000
_diffrn_orient_matrix_UB_32      0.0651245000
_diffrn_orient_matrix_UB_33      -0.0039548000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11955
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.342
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37195
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.2444
_exptl_crystal_size_mid          0.1027
_exptl_crystal_size_min          0.0518
_refine_diff_density_max         1.133
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4476
_reflns_number_total             6103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02683_si_002.cif
_cod_data_source_block           1
_cod_database_code               4349353
_manchester_internal_coll_name   adpm213
_manchester_internal_coll_client JJL/FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 15s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   29/05/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 29/06/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 29/06/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 30/06/2015
_manchester_internal_validation_user FO
_manchester_internal_validation_date 16/08/2015
_manchester_internal_archive_date 16/08/2015
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'La C50 N2'
_reflns_odcompleteness_completeness 99.70
_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. Rigid body (RIGU) restrains
 C21, C20, C19, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C6, C9, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C27(H27), C28(H28),
 C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'