Tunable ligand emission of napthylsalophen triple-decker dinuclear lanthanide(iii) sandwich complexes.
Hardy, E. E.; Wyss, K. M.; Keller, R. J.; Gorden, J. D.; Gorden, A. E. V.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1337–1346; doi:10.1039/c7dt03733c

data_7702158
_publ_section_title
;
 Tunable ligand emission of napthylsalophen triple-decker dinuclear
 lanthanide(iii) sandwich complexes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1337
_journal_page_last               1346
_journal_paper_doi               10.1039/c7dt03733c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C85 H58 N6 O7 Tb2'
_chemical_formula_sum            'C85 H58 N6 O7 Tb2'
_chemical_formula_weight         1593.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-10 deposited with the CCDC.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4934(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4947(6)
_cell_length_b                   20.5096(7)
_cell_length_c                   20.6071(7)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.34
_cell_volume                     7346.6(4)
_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 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_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  0.0498
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            107251
_diffrn_reflns_theta_full        27.0975
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1048 before and 0.0683 after correction. The Ratio of minimum to maximum transmission is 0.7767. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.4404
_exptl_crystal_description       block
_exptl_crystal_F_000             3184.5520
_exptl_crystal_recrystallization_method 'slow evaporation of DCM and Methanol'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.0405
_refine_diff_density_min         -1.3523
_refine_diff_density_rms         0.1730
_refine_ls_d_res_high            0.7802
_refine_ls_d_res_low             17.3825
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0780
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    113
_refine_ls_number_parameters     901
_refine_ls_number_reflns         16189
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0779
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          5.6845
_refine_ls_shift/su_mean         0.0150
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0023P)^2^+58.6398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                13926
_reflns_number_total             16189
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt03733c2.cif
_cod_data_source_block           Tb2L3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7702158
_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, All O(H) groups
2. Restrained distances
 O7-H7a
 0.87 with sigma of 0.01
 C85-H7a
 1.888164 with sigma of 0.02
 Tb2-H7a
 2.966988 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C46(H46), C74(H74), C54(H54), C21(H21), C77(H77), C18(H18), C41(H41),
 C72(H72), C44(H44), C30(H30), C82(H82), C11(H11), C67(H67), C34(H34), C26(H26),
  C16(H16), C69(H69), C36(H36), C31(H31), C64(H64), C59(H59), C55(H55),
 C78(H78), C3(H3), C13(H13), C42(H42), C58(H58), C83(H83), C15(H15), C2(H2),
 C24(H24), C27(H27), C70(H70), C63(H63), C71(H71), C23(H23), C5(H5), C8(H8),
 C14(H14), C7(H7), C43(H43), C35(H35), C33(H33), C62(H62), C6(H6), C22(H22),
 C61(H61), C80(H80), C52(H52), C79(H79), C51(H51), C49(H49), C50(H50), C39(H39)
3.b Idealised Me refined as rotating group:
 C85(H85a,H85b,H85c)
;
_olex2_exptl_crystal_mounting_method
'a suitable crystal was mounted on a glass fiber using n-paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'