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_4349358
_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         'C32 H40 K2 N4 O3, C4 H8 O'
_chemical_formula_sum            'C36 H48 K2 N4 O4'
_chemical_formula_weight         678.98
_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             2015-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                82.22(3)
_cell_angle_beta                 88.66(3)
_cell_angle_gamma                76.64(2)
_cell_formula_units_Z            2
_cell_length_a                   7.578(2)
_cell_length_b                   12.283(4)
_cell_length_c                   19.570(7)
_cell_measurement_reflns_used    796
_cell_measurement_temperature    150.02(11)
_cell_measurement_theta_max      21.0520
_cell_measurement_theta_min      3.7100
_cell_volume                     1755.9(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.02(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -65.00  -29.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -57.0000  -60.0000 36

  2 omega  -88.00   12.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663  -77.0000 -150.0000 100

  3 omega    9.00   61.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -99.0000  120.0000 52

  4 omega  -53.00   92.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601    0.0000   30.0000 145

  5 omega  -12.00   46.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -77.0000    0.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0222143000
_diffrn_orient_matrix_UB_12      0.0449033000
_diffrn_orient_matrix_UB_13      0.0146745000
_diffrn_orient_matrix_UB_21      0.0194182000
_diffrn_orient_matrix_UB_22      -0.0353709000
_diffrn_orient_matrix_UB_23      0.0319764000
_diffrn_orient_matrix_UB_31      0.0915678000
_diffrn_orient_matrix_UB_32      -0.0178748000
_diffrn_orient_matrix_UB_33      -0.0100253000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1741
_diffrn_reflns_av_unetI/netI     0.4737
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12116
_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         25.350
_diffrn_reflns_theta_min         3.383
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       needle
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.3788
_exptl_crystal_size_mid          0.0888
_exptl_crystal_size_min          0.0634
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6410
_refine_ls_number_restraints     618
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.3122
_refine_ls_R_factor_gt           0.1067
_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^)+(0.0691P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2141
_refine_ls_wR_factor_ref         0.2996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2021
_reflns_number_total             6410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02683_si_002.cif
_cod_data_source_block           6
_cod_database_code               4349358
_manchester_internal_coll_name   adpm117
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 35s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   13/01/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 16/01/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 16/01/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 17/08/2015
_manchester_internal_validation_user FO
_manchester_internal_validation_date 17/08/2015
_manchester_internal_archive_date 17/08/2015
_chemical_oxdiff_formula         'C20 H16 N4 K2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O4A-C36
 1.45 with sigma of 0.02
 O4-C33
 1.45 with sigma of 0.02
 C30A-C29 \\sim C29-C30 \\sim C31-C32 \\sim C36-C35 \\sim C33-C34 \\sim C22-C21
 with sigma of 0.02
 C22-C23 \\sim C27-C26 \\sim C31-C30 \\sim C30A-C31 \\sim C34-C35
 with sigma of 0.02
 O4A-C36 \\sim O4A-C33 \\sim O4-C36 \\sim O4-C33 \\sim O3-C29 \\sim O3-C32
\\sim O2-C28 \\sim O2-C25 \\sim O1-
 C21 \\sim O1-C24
 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(H29C)=Sof(H29D)=Sof(H31C)=Sof(H31D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(H31A)=Sof(H31B)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(1)
 Sof(O4A)=1-FVAR(2)
 Sof(O4)=FVAR(2)
 Fixed Sof: H33A(0.5) H33B(0.5) H33C(0.5) H33D(0.5) H36A(0.5) H36B(0.5)
 H36C(0.5) H36D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C29(H29C,H29D), C31(H31A,H31B), C31(H31C,H31D), C32(H32A,H32B), C30(H30A,H30B),
  C30A(H30C,H30D), C33(H33A,H33B), C33(H33C,H33D), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C36(H36C,H36D)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              62243
_shelx_hkl_checksum              20333
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'