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_7123728
_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 Er N8 O2, C F3 O3 S, C2 H5 O'
_chemical_formula_sum            'C47 H51 Er F3 N8 O6 S'
_chemical_formula_weight         1080.28
_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             2018-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-01-18 deposited with the CCDC.    2019-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.6743(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.8628(4)
_cell_length_b                   9.29634(17)
_cell_length_c                   37.5992(5)
_cell_measurement_reflns_used    29905
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.3890
_cell_measurement_theta_min      2.6650
_cell_volume                     9282.1(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      100.00(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 1.000
_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     35.00  90.00   1.00   20.00    --   18.18 178.00 -30.00   55
  2  \w    -49.00  35.00   1.00   20.00    --   18.18 -57.00   0.00   84
  3  \w     -1.00  87.00   1.00   20.00    --   18.18  38.00 -30.00   88
  4  \w     -1.00  87.00   1.00   20.00    --   18.18  38.00 150.00   88
  5  \w     -1.00  81.00   1.00   20.00    --   18.18  38.00  60.00   82
  6  \w    -88.00 -37.00   1.00   20.00    --  -18.49 152.00  40.00   51
;
_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      0.0075670000
_diffrn_orient_matrix_UB_12      0.0238911000
_diffrn_orient_matrix_UB_13      0.0179165000
_diffrn_orient_matrix_UB_21      -0.0160203000
_diffrn_orient_matrix_UB_22      -0.0518771000
_diffrn_orient_matrix_UB_23      0.0062309000
_diffrn_orient_matrix_UB_31      0.0199969000
_diffrn_orient_matrix_UB_32      -0.0505826000
_diffrn_orient_matrix_UB_33      0.0020594000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            39160
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.015
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.518
_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    1.546
_exptl_crystal_description       plate
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.563
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0170P)^2^+53.7207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7700
_reflns_number_total             8832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03934a2.cif
_cod_data_source_block           kma259
_cod_database_code               7123728
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C47H51Er1F3N8O6S
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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), C46(H46A,H46B)
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), C47(H47A,H47B,
 H47C)
;
_shelx_res_checksum              24559
_olex2_date_sample_data_collection 2018-04-28
_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 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.783