Th(IV) and Ce(IV) Napthylsalophen Sandwich Complexes: Characterization of Unusual Thorium Fluorescence in Solution and Solid-state
Hardy, Emily Elizabeth; Wyss, Kevin M.; Gorden, John D.; Ariyarathna, Isuru R.; Miliordos, Evangelos; Gorden, Anne E. V.; Chem. Commun.  (2017) –; doi:10.1039/C7CC06868A

data_7120762
_publ_section_title
;
 Th(IV) and Ce(IV) Napthylsalophen Sandwich Complexes: Characterization of
 Unusual Thorium Fluorescence in Solution and Solid-state
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06868A
_journal_year                    2017
_chemical_formula_moiety         'C56 H36 N4 O4 Th, C7 H8, C3.5 H3.5'
_chemical_formula_sum            'C66.5 H47.5 N4 O4 Th'
_chemical_formula_weight         1198.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-05-05 deposited with the CCDC.
2017-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                106.2207(11)
_cell_angle_beta                 90.8257(11)
_cell_angle_gamma                94.1515(11)
_cell_formula_units_Z            2
_cell_length_a                   11.4987(3)
_cell_length_b                   14.3617(4)
_cell_length_c                   16.2769(5)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      21.022
_cell_measurement_theta_min      2.166
_cell_volume                     2572.52(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9953
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59819
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.955
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0999 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.7609.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5474
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1180.2268
_exptl_crystal_recrystallization_method
'layered diffusion of hexanes into a saturated toluene solution'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.5980
_refine_diff_density_min         -1.7340
_refine_diff_density_rms         0.1940
_refine_ls_d_res_high            0.8100
_refine_ls_d_res_low             15.6187
_refine_ls_goodness_of_fit_ref   1.0413
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    94
_refine_ls_number_parameters     686
_refine_ls_number_reflns         10098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0413
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8478
_reflns_number_total             10098
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7cc06868a2.cif
_cod_data_source_block           Emily100316_ThL2
_cod_database_code               7120762
_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: C67S(0.5) H67a(0.5) H67b(0.5) H67c(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C43(H43), C42(H42), C41(H41), C2(H2), C3(H3), C55(H55), C54(H54),
 C31(H31), C30(H30), C27(H27), C26(H26), C16(H16), C15(H15), C14(H14), C13(H13),
  C8(H8), C7(H7), C6(H6), C5(H5), C52(H52), C51(H51), C50(H50), C49(H49),
 C36(H36), C35(H35), C34(H34), C33(H33), C21(H21), C22(H22), C23(H23), C24(H24),
  C61S(H61S), C60S(H60S), C59S(H59S), C58S(H58S), C57S(H57S), C11(H11),
 C18(H18), C39(H39), C46(H46), C66S(H66S), C65S(H65S)
3.b Idealised Me refined as rotating group:
 C63S(H63a,H63b,H63c), C67S(H67a,H67b,H67c)
;
_olex2_exptl_crystal_mounting_method
'suitable crystal was mounted on a glass fibre using paratone-n oil'
_olex2_submission_special_instructions 'No special instructions were received'