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_4349360
_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         'C80 H98 Ce2 O4 Si6, C7 H8'
_chemical_formula_sum            'C87 H106 Ce2 O4 Si6'
_chemical_formula_weight         1664.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.879(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1853(7)
_cell_length_b                   19.5732(6)
_cell_length_c                   21.1347(7)
_cell_measurement_reflns_used    12322
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.4206
_cell_measurement_theta_min      3.1530
_cell_volume                     8292.3(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega   70.71  243.71   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8669  329.2088 173

  2 phi    -25.16  274.03   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 106.1694   95.0000   73.8669     -     299

  3 phi    -25.79  188.34   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 228.1494  105.0000   73.8669     -     214

  4 phi      6.50  333.70   1.0006   10.0000
omega____ theta____ kappa____ phi______ frames
 259.2097  113.0000   73.8669     -     327

  5 omega  -60.34  123.66   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.0000   73.8669  131.7094 184

  6 phi   -120.64   76.48   1.0006    7.5000
omega____ theta____ kappa____ phi______ frames
 292.5994  -69.5000   73.8669     -     197

  7 omega   91.89  248.89   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8669  249.2094 157

  8 omega  119.92  235.92   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.0000   73.8669   99.2081 116

  9 omega  146.24  239.24   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669  174.2088 93
;
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'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0483662000
_diffrn_orient_matrix_UB_12      0.0443326000
_diffrn_orient_matrix_UB_13      0.0232750000
_diffrn_orient_matrix_UB_21      0.0527148000
_diffrn_orient_matrix_UB_22      0.0061891000
_diffrn_orient_matrix_UB_23      0.0698698000
_diffrn_orient_matrix_UB_31      0.0280938000
_diffrn_orient_matrix_UB_32      0.0646887000
_diffrn_orient_matrix_UB_33      -0.0227511000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1077
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24933
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.156
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+27.4646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5631
_reflns_number_total             7431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02683_si_002.cif
_cod_data_source_block           8
_cod_database_code               4349360
_manchester_internal_coll_name   xdpm31
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time '7.5 and 10s'
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w and \p scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   10/03/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 10/03/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 10/03/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 10/03/2015
_manchester_internal_validation_user FO
_manchester_internal_validation_date 24/11/2015
_manchester_internal_archive_date 24/11/2015
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.762
_reflns_odcompleteness_completeness 94.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.42
_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. Others
 Fixed Sof: H45A(0.5) H45B(0.5) H45C(0.5)
 Fixed U12: C41(0) C44(0) C45(0)
 Fixed U23: C41(0) C44(0) C45(0)
 Fixed X: C41(0.5) C44(0.5) C45(0.5)
 Fixed Z: C41(0.25) C44(0.25) C45(0.25)
3.a Ternary CH refined with riding coordinates:
 C32(H32)
3.b Me refined with riding coordinates:
 C45(H45A,H45B,H45C)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C33(H33), C34(H34),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44)
3.d 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)
;
_shelx_res_checksum              87389
_shelx_hkl_checksum              94770
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'