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_7123729
_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 O2 Yb, C F3 O3 S, C2 H5 O'
_chemical_formula_sum            'C47 H51 F3 N8 O6 S Yb'
_chemical_formula_weight         1086.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-16
_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                 131.202(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   49.2884(8)
_cell_length_b                   9.28670(10)
_cell_length_c                   26.8502(4)
_cell_measurement_reflns_used    59044
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.2870
_cell_measurement_theta_min      3.3180
_cell_volume                     9246.9(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -54.00  30.00   1.00    3.00    --  -37.09  57.00 150.00   84
  2  \w    -54.00  30.00   1.00    3.00    --  -37.09  57.00  90.00   84
  3  \w    -66.00  34.00   1.00    3.00    --  -37.09  19.00   0.00  100
  4  \w    -54.00  30.00   1.00    3.00    --  -37.09  57.00-120.00   84
  5  \w    -56.00  32.00   1.00    3.00    --  -37.09  38.00   0.00   88
  6  \w   -106.00  32.00   1.00    3.00    --  -37.09   0.00-120.00  138
  7  \w    -66.00  34.00   1.00    3.00    --  -37.09  19.00-120.00  100
  8  \w   -105.00 -10.00   1.00    3.00    --  -37.09 -77.00-120.00   95
  9  \w     23.00  90.00   1.00    3.00    --   37.09-125.00 -30.00   67
 10  \w     23.00  90.00   1.00    3.00    --   37.09-125.00-180.00   67
 11  \w     20.00 104.00   1.00    3.00    --   37.09  57.00  60.00   84
 12  \w     23.00  90.00   1.00    3.00    --   37.09-125.00  60.00   67
 13  \w     23.00  90.00   1.00    3.00    --   37.09-125.00 120.00   67
 14  \w     23.00  90.00   1.00    3.00    --   37.09-125.00  90.00   67
 15  \w      1.00  76.00   1.00    3.00    --   37.09 -99.00-180.00   75
 16  \w     23.00  90.00   1.00    3.00    --   37.09-125.00  30.00   67
 17  \w     23.00  90.00   1.00    3.00    --   37.09-125.00 150.00   67
 18  \w     84.00 178.00   1.00   15.00    --  111.00  77.00  90.00   94
 19  \w     44.00 129.00   1.00   15.00    --  111.00 -61.00 120.00   85
 20  \w     93.00 178.00   1.00   15.00    --  111.00  61.00 -90.00   85
 21  \w     41.00 132.00   1.00   15.00    --  111.00 -30.00 -60.00   91
 22  \w     93.00 178.00   1.00   15.00    --  111.00  61.00 -30.00   85
 23  \w     41.00 116.00   1.00   15.00    --  111.00-111.00 -60.00   75
 24  \w    100.00 178.00   1.00   15.00    --  111.00 111.00   0.00   78
 25  \w     42.00 109.00   1.00   15.00    --  111.00 -94.00 120.00   67
 26  \w     41.00 132.00   1.00   15.00    --  111.00 -30.00 120.00   91
 27  \w     94.00 178.00   1.00   15.00    --  111.00  45.00-180.00   84
 28  \w     90.00 178.00   1.00   15.00    --  111.00  30.00-120.00   88
 29  \w     44.00 129.00   1.00   15.00    --  111.00 -61.00-120.00   85
 30  \w     41.00 116.00   1.00   15.00    --  111.00-111.00-180.00   75
 31  \w     90.00 178.00   1.00   15.00    --  111.00  30.00 150.00   88
 32  \w     41.00 116.00   1.00   15.00    --  111.00-111.00  90.00   75
 33  \w     42.00 109.00   1.00   15.00    --  111.00 -94.00-150.00   67
 34  \w     41.00 116.00   1.00   15.00    --  111.00-111.00  30.00   75
 35  \w     57.00 150.00   1.00   15.00    --  111.00 178.00 120.00   93
 36  \w     43.00 128.00   1.00   15.00    --  111.00 -45.00-180.00   85
 37  \w    100.00 178.00   1.00   15.00    --  111.00 111.00-150.00   78
 38  \w    -64.00  30.00   1.00    3.00    --  -37.09  77.00 -90.00   94
 39  \w   -105.00 -10.00   1.00    3.00    --  -37.09 -77.00 -60.00   95
 40  \w   -108.00  -8.00   1.00    3.00    --  -37.09 -19.00 120.00  100
 41  \w     10.00 105.00   1.00    3.00    --   37.09  77.00  60.00   95
 42  \w      8.00 108.00   1.00    3.00    --   37.09  19.00-120.00  100
 43  \w     20.00 104.00   1.00    3.00    --   37.09  57.00 150.00   84
 44  \w     18.00 106.00   1.00    3.00    --   37.09  38.00 -30.00   88
 45  \w     18.00 106.00   1.00    3.00    --   37.09  38.00  60.00   88
 46  \w     20.00 104.00   1.00    3.00    --   37.09  57.00-120.00   84
 47  \w     10.00 105.00   1.00    3.00    --   37.09  77.00-120.00   95
 48  \w     10.00 105.00   1.00    3.00    --   37.09  77.00-180.00   95
 49  \w     10.00 105.00   1.00    3.00    --   37.09  77.00 -30.00   95
 50  \w     10.00 105.00   1.00    3.00    --   37.09  77.00  90.00   95
 51  \w     20.00 104.00   1.00    3.00    --   37.09  57.00   0.00   84
 52  \w     18.00 106.00   1.00    3.00    --   37.09  38.00-120.00   88
 53  \w     10.00 105.00   1.00    3.00    --   37.09  77.00 150.00   95
;
_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      0.0064395000
_diffrn_orient_matrix_UB_12      -0.0454712000
_diffrn_orient_matrix_UB_13      -0.0466740000
_diffrn_orient_matrix_UB_21      -0.0028987000
_diffrn_orient_matrix_UB_22      0.1584719000
_diffrn_orient_matrix_UB_23      -0.0199649000
_diffrn_orient_matrix_UB_31      0.0409378000
_diffrn_orient_matrix_UB_32      0.0183612000
_diffrn_orient_matrix_UB_33      0.0569057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0110
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            85837
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.590
_diffrn_reflns_theta_min         3.330
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.752
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.733
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_recrystallization_method 'from 1,2-dimethoxyethane/diethyl ether'
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.572
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         9275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+66.4582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9108
_reflns_number_total             9275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03934a2.cif
_cod_data_source_block           kma363
_cod_original_cell_volume        9246.9(4)
_cod_database_code               7123729
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C47H51.5F3N8O6SYb
_reflns_odcompleteness_completeness 99.96
_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.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C39(H39A,H39B), C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C11(H11), C13(H13),
 C14(H14), C19(H19), C20(H20), C21(H21), C22(H22), C27(H27), C28(H28), C29(H29),
  C30(H30), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42),
 C43(H43), C44(H44)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C46(H46A,H46B,
 H46C)
;
_shelx_res_checksum              33452
_olex2_date_sample_data_collection 2018-12-15
_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 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.878