Highly luminescent lanthanide complexes sensitised by tertiary amide-linked carbostyril antennae.
Kovacs, Daniel; Phipps, Dulcie; Orthaber, Andreas; Borbas, K. Eszter; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10702–10714; doi:10.1039/c8dt01270a

data_7046672
_publ_section_title
;
 Highly luminescent lanthanide complexes sensitised by tertiary
 amide-linked carbostyril antennae.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10702
_journal_page_last               10714
_journal_paper_doi               10.1039/c8dt01270a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C30 H41 Dy N6 O11'
_chemical_formula_sum            'C30 H41 Dy N6 O11'
_chemical_formula_weight         824.19
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2018-06-07 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                100.1990(10)
_cell_angle_beta                 98.0780(10)
_cell_angle_gamma                107.4760(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7962(2)
_cell_length_b                   14.4010(4)
_cell_length_c                   17.6620(5)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.34
_cell_measurement_theta_min      2.39
_cell_volume                     2055.14(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2  (Bruker AXS, 2012)'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46688
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.877
_diffrn_reflns_theta_min         1.706
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1018 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.8053.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.630
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         12686
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10870
_reflns_number_total             12686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01270a2.cif
_cod_data_source_block           ao_keb_dk_dy_glyme_1_0m_a
_cod_depositor_comments
'Adding full bibliography for 7046671--7046672.cif.'
_cod_original_cell_volume        2055.13(9)
_cod_database_code               7046672
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B
 0.95 with sigma of 0.1
3. Others
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(C15B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C28(H28A,H28B), C24(H24A,H24B), C30(H30A,H30B), C27(H27A,
 H27B), C22(H22A,H22B), C26(H26A,H26B), C20(H20A,H20B), C25(H25A,H25B),
 C23(H23A,H23B), C19(H19A,H19B), C12(H12A,H12B), C32(H32A,H32B), C14(H14A,H14B),
  C14(H14C,H14D)
4.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C15B(H15A,H15B,H15C), C15A(H15D,H15E,H15F)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C5(H5), C8(H8), C6(H6)
;
_shelx_fab_checksum              24338
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'