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_4349357
_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         'C52 H84 I2 La2'
_chemical_formula_sum            'C52 H84 I2 La2'
_chemical_formula_weight         1240.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                90.556(3)
_cell_angle_beta                 98.291(3)
_cell_angle_gamma                104.438(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5116(3)
_cell_length_b                   11.3423(4)
_cell_length_c                   23.8269(11)
_cell_measurement_reflns_used    7547
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      28.7140
_cell_measurement_theta_min      3.7030
_cell_volume                     2719.22(18)
_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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.02(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -16.00   91.00   1.0000    4.6700
omega____ theta____ kappa____ phi______ frames
    -       18.8601   19.0000    0.0000 107

  2 omega   31.00   64.00   1.0000    4.6700
omega____ theta____ kappa____ phi______ frames
    -       18.8601 -114.0000  -28.0000 33

  3 omega   -5.00   21.00   1.0000    4.6700
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000 -120.0000 26

  4 omega  -50.00   39.00   1.0000    4.6700
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -57.0000 -180.0000 89

  5 omega  -11.00   29.00   1.0000    4.6700
omega____ theta____ kappa____ phi______ frames
    -       18.8601   77.0000 -180.0000 40

  6 omega  -18.00    7.00   1.0000    4.6700
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  114.0000   61.0000 25

  7 omega  -20.00   61.00   1.0000    4.6700
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000   60.0000 81
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0069928000
_diffrn_orient_matrix_UB_12      0.0225576000
_diffrn_orient_matrix_UB_13      0.0284450000
_diffrn_orient_matrix_UB_21      0.0467659000
_diffrn_orient_matrix_UB_22      -0.0344179000
_diffrn_orient_matrix_UB_23      0.0084249000
_diffrn_orient_matrix_UB_31      0.0522781000
_diffrn_orient_matrix_UB_32      0.0498597000
_diffrn_orient_matrix_UB_33      -0.0051928000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            22794
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.299
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.926
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.1555
_exptl_crystal_size_mid          0.0825
_exptl_crystal_size_min          0.0653
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.297
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         9938
_refine_ls_number_restraints     780
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0658
_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^)+34.0823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7928
_reflns_number_total             9938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02683_si_002.cif
_cod_data_source_block           5
_cod_original_cell_volume        2719.24(18)
_cod_database_code               4349357
_manchester_internal_coll_name   adpm176
_manchester_internal_coll_client JJL/FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 4.67s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   19/05/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 15/06/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 15/06/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 15/06/2015
_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         'La2 C30 I2 H70'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9087(13) 0.0913(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C11(H11), C13(H13), C14(H14), C24(H24), C26(H26),
 C27(H27), C37(H37), C39(H39), C40(H40)
4.b Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C35(H35A,H35B,H35C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C68(H68A,
 H68B,H68C), C88(H88A,H88B,H88C)
;
_olex2_submission_special_instructions 'No special instructions were received'