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_7702161
_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 Yb2'
_chemical_formula_sum            'C85 H58 N6 O7 Yb2'
_chemical_formula_weight         1621.52
_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             2017-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2707(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4078(8)
_cell_length_b                   20.4235(10)
_cell_length_c                   20.6623(10)
_cell_measurement_reflns_used    9412
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.33
_cell_measurement_theta_min      2.19
_cell_volume                     7302.1(6)
_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
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9999
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            100866
_diffrn_reflns_theta_full        26.0222
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.605
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0994 before and 0.0556 after correction. The Ratio of minimum to maximum transmission is 0.8004. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4749
_exptl_crystal_description       block
_exptl_crystal_F_000             3223.6040
_exptl_crystal_recrystallization_method
'slow evaporation dicloromethane methanol'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.2627
_refine_diff_density_min         -1.4599
_refine_diff_density_rms         0.2024
_refine_ls_d_res_high            0.8100
_refine_ls_d_res_low             14.4821
_refine_ls_goodness_of_fit_ref   1.0757
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    113
_refine_ls_number_parameters     905
_refine_ls_number_reflns         14394
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0756
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0000P)^2^+53.8387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                12656
_reflns_number_total             14394
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt03733c2.cif
_cod_data_source_block           Emily111016_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7702161
_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-H8a
 0.87 with sigma of 0.01
 C85-H8a
 1.892946 with sigma of 0.02
 Yb1-H8a
 2.888746 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C22(H39), C61(H18), C21(H40), C2(H33), C78(H8), C77(H9), C27(H35), C24(H37),
 C64(H22), C3(H32), C5(H30), C6(H31), C62(H20), C8(H27), C83(H3), C79(H7),
 C82(H4), C7(H26), C80(H6), C26(H34), C59(H16), C23(H38), C71(H24), C49(H25),
 C63(H21), C14(H47), C16(H45), C15(H46), C13(H48), C50(H55), C69(H56), C74(H58),
  C67(H57), C52(H53), C51(H54), C18(H50), C55(H59), C54(H60), C44(H64),
 C43(H65), C41(H67), C72(H66), C42(H68), C70(H72), C30(H84), C39(H75), C35(H79),
  C34(H80), C33(H81), C36(H78), C31(H83), C46(H91), C11(H92), C58(H93)
3.b Idealised Me refined as rotating group:
 C85(H87a,H87b,H87c)
;
_smtbx_masks_special_details
'each void contains one disordered DCM and one disorded water molecule'
_olex2_exptl_crystal_mounting_method
'Suitable crystal was selected and mounted on a glass fiber using n-paratone oil.'
_olex2_submission_special_instructions 'No special instructions were received'