Monometallic lanthanide salicylhydrazone complexes exhibiting strong near-infrared luminescence
Ayers, Kaitlynn M.; Schley, Nathan D.; Ung, Gaël; Chemical Communications  (2019) –; doi:10.1039/C9CC03934A

data_7123727
_publ_section_title
;
 Monometallic lanthanide salicylhydrazone complexes exhibiting strong
 near-infrared luminescence
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03934A
_journal_year                    2019
_chemical_formula_moiety         'C44 H46 N8 Nd O2, C F3 O3 S, 0.5(C4 O1)'
_chemical_formula_sum            'C47 H46 F3 N8 Nd O5.5 S'
_chemical_formula_weight         1044.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-18 deposited with the CCDC.    2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.8320(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.8547(6)
_cell_length_b                   9.37739(14)
_cell_length_c                   26.6795(4)
_cell_measurement_reflns_used    16266
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.0540
_cell_measurement_theta_min      3.3350
_cell_volume                     9382.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -104.00 -20.00   1.00    8.00    --  -37.09 -57.00 150.00   84
  2  \w   -104.00 -20.00   1.00    8.00    --  -37.09 -57.00  60.00   84
  3  \w    -30.00  64.00   1.00    8.00    --   37.09 -77.00-150.00   94
  4  \w    -30.00  54.00   1.00    8.00    --   37.09 -57.00  90.00   84
  5  \w    -30.00  54.00   1.00    8.00    --   37.09 -57.00-150.00   84
  6  \w      8.00 108.00   1.00    8.00    --   37.09  19.00-150.00  100
  7  \w     20.00 104.00   1.00    8.00    --   37.09  57.00   0.00   84
  8  \w     43.00 139.00   1.00   24.00    --  111.00 -80.00 -72.37   96
  9  \w     43.00 138.00   1.00   24.00    --  111.00 -77.00   0.00   95
 10  \w     41.00 132.00   1.00   24.00    --  111.00 -30.00  30.00   91
 11  \w     41.00 132.00   1.00   24.00    --  111.00 -30.00 -30.00   91
 12  \w     93.00 178.00   1.00   24.00    --  111.00  61.00 -60.00   85
 13  \w     90.00 178.00   1.00   24.00    --  111.00  30.00 -90.00   88
 14  \w     41.00 132.00   1.00   24.00    --  111.00 -30.00-120.00   91
 15  \w     43.00 139.00   1.00   24.00    --  111.00 -80.00 138.48   96
 16  \w    -64.00  30.00   1.00    8.00    --  -37.09  77.00  30.00   94
 17  \w    -64.00 -16.00   1.00    8.00    --  -37.09  77.00 120.00   48
 18  \w   -105.00 -10.00   1.00    8.00    --  -37.09 -77.00 -30.00   95
 19  \w   -105.00 -10.00   1.00    8.00    --  -37.09 -77.00-120.00   95
 20  \w   -105.00 -10.00   1.00    8.00    --  -37.09 -77.00  30.00   95
 21  \w    -30.00  54.00   1.00    8.00    --   37.09 -57.00 -90.00   84
 22  \w     20.00 104.00   1.00    8.00    --   37.09  57.00 -90.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0006855000
_diffrn_orient_matrix_UB_12      -0.0416752000
_diffrn_orient_matrix_UB_13      0.0559754000
_diffrn_orient_matrix_UB_21      0.0410702000
_diffrn_orient_matrix_UB_22      0.0039935000
_diffrn_orient_matrix_UB_23      0.0073219000
_diffrn_orient_matrix_UB_31      -0.0008480000
_diffrn_orient_matrix_UB_32      0.1588501000
_diffrn_orient_matrix_UB_33      0.0145224000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35768
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.724
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.428
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       plate
_exptl_crystal_F_000             4248
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.359
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         9266
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+11.3988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7734
_reflns_number_total             9266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03934a2.cif
_cod_data_source_block           kma311
_cod_original_formula_sum        'C47 H46 F3 N8 Nd O5.50 S'
_cod_database_code               7123727
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C47H52F3N8NdO5S
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.252
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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) groups
2. Uiso/Uaniso restraints and constraints
O6 \\sim O6B \\sim C46 \\sim C46B \\sim C47 \\sim C47B \\sim C48 \\sim C48B
\\sim C49 \\sim C49B: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
3. Others
 1*[Sof(O6B)+Sof(C46B)+Sof(C47B)+Sof(C48B)+Sof(C49B)]+1*[Sof(O6)+Sof(C46)+
 Sof(C47)+Sof(C48)+Sof(C49)]=0.5 with esd of 0.0001
 Sof(O6B)=Sof(C46B)=Sof(C47B)=Sof(C48B)=Sof(C49B)=FVAR(1)
 Sof(O6)=Sof(C46)=Sof(C47)=Sof(C48)=Sof(C49)=FVAR(2)
4.a Free rotating group:
 O6(C46,C47,C48,C49), O6B(C46B,C47B,C48B,C49B)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C21(H21A,H21B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C36(H36), C37(H37),
 C39(H39), C40(H40)
4.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              2890
_olex2_date_sample_data_collection 2018-10-11
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.039
_oxdiff_exptl_absorpt_empirical_full_min 0.694