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_4349354
_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 Ce N2'
_chemical_formula_sum            'C36 H50 Ce N2'
_chemical_formula_weight         650.90
_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             2015-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.121(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5750(11)
_cell_length_b                   10.6089(5)
_cell_length_c                   19.2302(9)
_cell_measurement_reflns_used    3798
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      27.8240
_cell_measurement_theta_min      3.6770
_cell_volume                     3293.2(3)
_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
;
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      120.01(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  -90.00  -46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.5548 -178.0000   90.0000 44

  2 omega   10.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6485  -99.0000   90.0000 56

  3 omega  -48.00   88.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       21.6485  -19.0000  -60.0000 136
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0308306000
_diffrn_orient_matrix_UB_12      0.0444580000
_diffrn_orient_matrix_UB_13      0.0155114000
_diffrn_orient_matrix_UB_21      0.0281585000
_diffrn_orient_matrix_UB_22      -0.0288837000
_diffrn_orient_matrix_UB_23      -0.0178013000
_diffrn_orient_matrix_UB_31      -0.0136596000
_diffrn_orient_matrix_UB_32      0.0407797000
_diffrn_orient_matrix_UB_33      -0.0296297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12002
_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         25.348
_diffrn_reflns_theta_min         3.356
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65867
_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 red'
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.1983
_exptl_crystal_size_mid          0.1577
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6007
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0516
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4551
_reflns_number_total             6007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02683_si_002.cif
_cod_data_source_block           2
_cod_database_code               4349354
_manchester_internal_coll_name   adpm169
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 5s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   15/5/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 18/05/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 18/05/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 16/08/2015
_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         'Ce N2 C38 H80'
_reflns_odcompleteness_completeness 99.69
_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. Restrained distances
 C21-C19 \\sim C21A-C19 \\sim C20A-C19 \\sim C20-C19 \\sim C19-C22A \\sim
C19-C22 \\sim C12-C10 \\sim C13-
 C10 \\sim C10-C11 \\sim C25-C23 \\sim C23-C24 \\sim C23-C26 \\sim C8-C6 \\sim
C9-C6 \\sim C7-C6
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C22A, C22, C21A, C21, C19, C20, C20A, C18, C17, C16, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C20)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21)=Sof(H21D)=Sof(H21E)=Sof(H21F)=
 Sof(C22)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21A)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
5.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)
5.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), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C),
 C22A(H22A,H22B,H22C), C20(H20D,H20E,H20F), C21(H21D,H21E,H21F), C22(H22D,H22E,
 H22F)
;
_olex2_submission_special_instructions 'No special instructions were received'