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_4349355
_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_absolute_configuration ad
_chemical_formula_moiety         'C32 H50 Ce N2 Si4'
_chemical_formula_sum            'C32 H50 Ce N2 Si4'
_chemical_formula_weight         715.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1559(2)
_cell_length_b                   17.1622(3)
_cell_length_c                   19.2840(3)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.32
_cell_measurement_theta_min      3.45
_cell_volume                     3692.11(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT A'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10822
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.924
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1257 before and 0.0780 after correction.
The Ratio of minimum to maximum transmission is 0.5707.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.144
_refine_diff_density_max         2.668
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                5302
_reflns_number_total             5472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02683_si_002.cif
_cod_data_source_block           3
_cod_database_code               4349355
_manchester_internal_coll_name   xdpm13
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time '10 & 25s'
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w and \p scans''
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   04/08/2014
_manchester_internal_process_user FO
_manchester_internal_process_date 14/08/2014
_manchester_internal_solution_user FO
_manchester_internal_solution_date 14/08/2014
_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
_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.a 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)
2.b 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), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              78531
_shelx_hkl_checksum              46332