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_7702160
_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 Ho2 N6 O7, 2(C H4 O)'
_chemical_formula_sum            'C87 H66 Ho2 N6 O9'
_chemical_formula_weight         1669.39
_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             2017-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                82.6930(6)
_cell_angle_beta                 86.1741(6)
_cell_angle_gamma                82.4147(6)
_cell_formula_units_Z            2
_cell_length_a                   10.3525(1)
_cell_length_b                   17.6031(2)
_cell_length_c                   18.9169(2)
_cell_measurement_reflns_used    9705
_cell_measurement_temperature    180.65
_cell_measurement_theta_max      30.440
_cell_measurement_theta_min      2.325
_cell_volume                     3385.05(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      180.65
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9985
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            127024
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         1.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.390
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0620 before and 0.0417 after correction.
The Ratio of minimum to maximum transmission is 0.8510.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.6377
_exptl_crystal_description       block
_exptl_crystal_F_000             1672.5761
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.2267
_refine_diff_density_min         -1.8970
_refine_diff_density_rms         0.1696
_refine_ls_d_res_high            0.6992
_refine_ls_d_res_low             13.5550
_refine_ls_goodness_of_fit_ref   1.1538
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    125
_refine_ls_number_parameters     944
_refine_ls_number_reflns         20696
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.1537
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0202P)^2^+5.2393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              25
_reflns_limit_k_min              -24
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                16856
_reflns_number_total             20696
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt03733c2.cif
_cod_data_source_block           NAK042017_0m
_cod_database_code               7702160
_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-H7
 0.87 with sigma of 0.01
 C85-H7
 1.863295 with sigma of 0.02
 Ho2-H7
 2.957705 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C55(H55), C46(H46), C30(H30), C72(H72), C74(H74), C67(H67), C39(H39),
 C54(H54), C18(H18), C13(H13), C44(H44), C11(H11), C69(H69), C31(H31), C71(H71),
  C83(H83), C41(H41), C43(H43), C36(H36), C6(H6), C16(H16), C82(H82), C77(H77),
 C70(H70), C42(H42), C78(H78), C21(H21), C52(H52), C22(H22), C2(H2), C58(H58),
 C3(H3), C8(H8), C27(H27), C26(H26), C15(H15), C49(H49), C62(H62), C5(H5),
 C59(H59), C80(H80), C14(H14), C24(H24), C33(H33), C23(H23), C63(H63), C79(H79),
  C7(H7a), C50(H50), C51(H51), C64(H64), C35(H35), C61(H61), C34(H34)
3.b Idealised Me refined as rotating group:
 C85(H85a,H85b,H85c), C86(H86a,H86b,H86c), C87(H87a,H87b,H87c)
3.c Idealised tetrahedral OH refined as rotating group:
 O8(H8a), O9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'