Mixed chelating ligands used to regulate the luminescence of Ln(iii) complexes and single-ion magnet behavior in Dy-based analogues.
Wang, Hai-Ling; Ma, Xiong-Feng; Zou, Hua-Hong; Wang, Kai; Li, Bo; Chen, Zi-Lu; Liang, Fu-Pei; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15929–15940; doi:10.1039/c8dt03133a

data_7047815
_publ_section_title
;
 Mixed chelating ligands used to regulate the luminescence of Ln(iii)
 complexes and single-ion magnet behavior in Dy-based analogues.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15929
_journal_page_last               15940
_journal_paper_doi               10.1039/c8dt03133a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C32 H20 Cl4 Er N5 O5'
_chemical_formula_sum            'C32 H20 Cl4 Er N5 O5'
_chemical_formula_weight         863.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.802(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2305(3)
_cell_length_b                   16.6540(3)
_cell_length_c                   14.3223(3)
_cell_measurement_reflns_used    11843
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9390
_cell_measurement_theta_min      3.9020
_cell_volume                     3126.57(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -22.00  87.00   1.00    5.00    --   10.68  77.00  30.00  109
  2  \w    -48.00  28.00   1.00    5.00    --   10.68 -77.00  60.00   76
  3  \w    -82.00  12.00   1.00    5.00    --  -11.93 -57.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0469025000
_diffrn_orient_matrix_UB_12      -0.0100949000
_diffrn_orient_matrix_UB_13      -0.0158745000
_diffrn_orient_matrix_UB_21      -0.0131506000
_diffrn_orient_matrix_UB_22      -0.0412592000
_diffrn_orient_matrix_UB_23      0.0004563000
_diffrn_orient_matrix_UB_31      -0.0235753000
_diffrn_orient_matrix_UB_32      0.0029755000
_diffrn_orient_matrix_UB_33      -0.0474047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22262
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+1.8862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0529
_reflns_number_gt                5233
_reflns_number_total             6131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt03133a2.cif
_cod_data_source_block           lfp_whl_1242aaaa
_cod_depositor_comments
'Adding full bibliography for 7047809--7047819.cif.'
_cod_database_code               7047815
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C29(H29), C3(H3), C2(H2), C9(H9), C8(H8), C15(H15),
 C19(H19), C25(H25), C16(H16), C26(H26), C6(H6), C5(H5)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C)
;
_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 1.540
_oxdiff_exptl_absorpt_empirical_full_min 0.751