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_7702155
_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 Gd2 N6 O7, 2(C H2 Cl2), C H4 O'
_chemical_formula_sum            'C88 H66 Cl4 Gd2 N6 O8'
_chemical_formula_weight         1791.85
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-20
_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.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                87.7454(8)
_cell_angle_beta                 75.9048(7)
_cell_angle_gamma                85.8045(7)
_cell_formula_units_Z            2
_cell_length_a                   12.3985(2)
_cell_length_b                   17.1412(3)
_cell_length_c                   17.7640(3)
_cell_measurement_reflns_used    9077
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      30.097
_cell_measurement_theta_min      2.29
_cell_volume                     3650.92(11)
_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 0.9995
_diffrn_measured_fraction_theta_max 0.9994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            112543
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.013
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1032 before and 0.0484 after correction. The Ratio of minimum to maximum transmission is 0.7519. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.6298
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1794.2318
_exptl_crystal_recrystallization_method
'slow evaporation of a saturated DCM/MeOH solution'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.2932
_refine_diff_density_min         -2.2968
_refine_diff_density_rms         0.1694
_refine_ls_d_res_high            0.7200
_refine_ls_d_res_low             17.0910
_refine_ls_goodness_of_fit_ref   1.1553
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    126
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         20486
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.1552
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.0105
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+15.0120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                16972
_reflns_number_total             20486
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt03733c2.cif
_cod_data_source_block           Emily120516_0m
_cod_database_code               7702155
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O7-H7
 0.87 with sigma of 0.01
 C85-H7
 1.861385 with sigma of 0.02
 Gd2-H7
 2.984588 with sigma of 0.02
3. Others
 Fixed Sof: C88A(0.5) H88a(0.5) H88b(0.5) C88B(0.5) H88c(0.5) H88d(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C87(H87a,H87b), C88A(H88a,H88b), C88B(H88c,H88d)
4.b Aromatic/amide H refined with riding coordinates:
 C71(H71), C46(H46), C39(H39), C67(H67), C58(H58), C72(H72), C82(H82),
 C30(H30), C77(H77), C74(H74), C44(H44), C54(H54), C55(H55), C41(H41), C70(H70),
  C78(H78), C31(H31), C11(H11), C18(H18), C13(H13), C49(H49), C79(H79),
 C69(H69), C83(H83), C26(H26), C51(H51), C59(H59), C80(H80), C16(H16), C5(H5),
 C21(H21), C61(H61), C15(H15), C2(H2), C27(H27), C43(H43), C64(H64), C3(H3),
 C24(H24), C36(H36), C50(H50), C8(H8), C6(H6), C42(H42), C22(H22), C14(H14),
 C62(H62), C63(H63), C52(H52), C33(H33), C35(H35), C7(H7a), C23(H23), C34(H34)
4.c Idealised tetrahedral OH refined as rotating group:
 O8(H8a)
;
_olex2_submission_special_instructions 'No special instructions were received'