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_7120761
_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 Ce N4 O4, O, 0.5(C6)'
_chemical_formula_sum            'C59 H36 Ce N4 O5'
_chemical_formula_weight         1021.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_audit_update_record
;
2016-12-20 deposited with the CCDC.
2017-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6888(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0103(8)
_cell_length_b                   13.9521(8)
_cell_length_c                   26.1970(15)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      28.217
_cell_measurement_theta_min      2.203
_cell_volume                     4687.5(5)
_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., 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            61172
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0959 before and 0.0417 after correction. The Ratio of minimum to maximum transmission is 0.8156. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orangish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.4468
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064.4438
_exptl_crystal_preparation
'slow diffusion of hexanes into a concentration solution in toluene'
_exptl_crystal_recrystallization_method
'slow diffusion of hexanes into a concentration solution in toluene'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.7761
_refine_diff_density_min         -0.6007
_refine_diff_density_rms         0.1251
_refine_ls_d_res_high            0.7900
_refine_ls_d_res_low             12.9117
_refine_ls_goodness_of_fit_ref   1.0683
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0683
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+3.6257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              -12
_reflns_number_gt                8118
_reflns_number_total             9966
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7cc06868a2.cif
_cod_data_source_block           Emily091116_0m
_cod_database_code               7120761
_olex2_refinement_description
;
;
_olex2_exptl_crystal_mounting_method
'mounted on a glass fibre using n-paratone oil '
_olex2_submission_special_instructions 'No special instructions were received'