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_4349359
_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         'C90 H120 Ce2 N4 O2 Si8'
_chemical_formula_sum            'C90 H120 Ce2 N4 O2 Si8'
_chemical_formula_weight         1794.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-09
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.663(4)
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_cell_length_c                   23.8999(8)
_cell_measurement_reflns_used    17855
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.7190
_cell_measurement_theta_min      2.2310
_cell_volume                     9502.1(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   74.31  257.01   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      103.9488   73.8669   29.3487 261

  2 omega -108.32   73.68   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -51.34  105.46   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.7963   73.8669   30.9163 224

  4 omega   70.51  253.21   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      100.1469   73.8669  113.7525 261

  5 omega   82.48  264.48   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      112.1209   73.8669  -22.6869 260

  6 omega  100.52  248.22   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      100.1559   73.8669 -143.5144 211

  7 phi   -145.34  209.88   0.7006   40.0000
omega____ theta____ kappa____ phi______ frames
 -42.5375  -31.7472   73.8669     -     507

  8 phi    -24.42  338.88   0.7000   40.0000
omega____ theta____ kappa____ phi______ frames
 -97.7494  104.0409   73.8669     -     519
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_diffrn_reflns_number            63216
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_diffrn_reflns_theta_full        67.497
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.255
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'w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+69.8588P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_number_gt                10881
_reflns_number_total             16978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02683_si_002.cif
_cod_data_source_block           7
_cod_original_cell_volume        9502.0(5)
_cod_database_code               4349359
_manchester_internal_coll_name   xdpm39
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 40s
_manchester_internal_coll_frame_width 0.7
_manchester_internal_coll_frame_method '\w and \p scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   03/07/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 06/07/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 06/07/2015
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_manchester_internal_refinement_date 10/07/2015
_manchester_internal_validation_user FO
_manchester_internal_validation_date 23/08/2015
_manchester_internal_archive_date 23/08/2015
_chemical_oxdiff_formula         C90H120Ce2N4O2Si8
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 Si6-C67 \\sim Si6-C69 \\sim Si6-C68 \\sim Si5-C64 \\sim Si5-C66 \\sim Si5-C65
\\sim Si8-C80 \\sim Si8-C79
 \\sim Si8-C78 \\sim Si7-C76 \\sim Si7-C75 \\sim Si7-C77 \\sim Si3-C18 \\sim
Si3-C19 \\sim Si3-C17 \\sim Si1-C8
 \\sim Si1-C6 \\sim Si1-C7 \\sim Si2-C9 \\sim Si2-C10 \\sim Si2-C11 \\sim
Si4-C21 \\sim Si4-C22 \\sim Si4-C20
 with sigma of 0.02
 Si7-C75 \\sim Si7-C76 \\sim Si7-C77 \\sim Si8-C79 \\sim Si8-C78 \\sim Si8-C80
\\sim Si5-C66 \\sim Si5-C64
 \\sim Si6-C68 \\sim Si6-C67 \\sim Si6-C69 \\sim Si4-C20 \\sim Si4-C22 \\sim
Si4-C21 \\sim Si2-C10 \\sim Si2-
 C11 \\sim Si2-C9 \\sim Si1-C8A \\sim Si1-C6 \\sim Si1-C8 \\sim Si1-C7A \\sim
Si1-C7 \\sim Si1-C6A \\sim Si3-
 C17 \\sim Si3-C18 \\sim Si3-C19 \\sim Si6-C68 \\sim Si6A-C68A \\sim Si6A-C67A
\\sim Si6-C67 \\sim Si6-C69
 \\sim Si7A-C77A \\sim Si7-C77 \\sim Si7-C75 \\sim Si7A-C75A \\sim Si7A-C76A
\\sim Si7-C76
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=
 Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(1)
 Sof(Si8A)=Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=Sof(C79A)=Sof(H79D)=
 Sof(H79E)=Sof(H79F)=Sof(C80A)=Sof(H80D)=Sof(H80E)=Sof(H80F)=1-FVAR(2)
 Sof(Si8)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C79)=Sof(H79A)=Sof(H79B)=
 Sof(H79C)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=FVAR(2)
 Sof(Si6A)=Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C68A)=Sof(H68D)=
 Sof(H68E)=Sof(H68F)=Sof(C69A)=Sof(H69D)=Sof(H69E)=Sof(H69F)=1-FVAR(3)
 Sof(Si6)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C68)=Sof(H68A)=Sof(H68B)=
 Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=FVAR(3)
 Sof(Si7A)=Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C76A)=Sof(H76D)=
 Sof(H76E)=Sof(H76F)=Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=1-FVAR(4)
 Sof(Si7)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C76)=Sof(H76A)=Sof(H76B)=
 Sof(H76C)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C43(H43)
5.b Me refined with riding coordinates:
 C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C75(H75A,H75B,
 H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C6A(H6AA,
 H6AB,H6AC), C67A(H67D,H67E,H67F), C68A(H68D,H68E,H68F), C69A(H69D,H69E,H69F),
 C75A(H75D,H75E,H75F), C76A(H76D,H76E,H76F), C77A(H77D,H77E,H77F)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C23(H23), C24(H24),
 C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45),
 C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C60(H60), C62(H62), C63(H63), C71(H71), C73(H73),
 C74(H74), C81(H81), C82(H82), C83(H83), C84(H84), C87(H87), C88(H88), C89(H89),
  C90(H90)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,
 H8AC), C78A(H78D,H78E,H78F), C79A(H79D,H79E,H79F), C80A(H80D,H80E,H80F)
;
_shelx_res_checksum              32489
_shelx_hkl_checksum              11193
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'