Regulation of the Metal Center and Coordinating Anion of Mononuclear Ln(III) Complexes to Promote an Efficient Luminescence Response to Various Organic Solvents
Wang, Hui-Feng; Ma, Xiong-Feng; Zhu, Zhong-Hong; Zou, Hua-Hong; Liang, Fu-Pei; Langmuir  (2020) –; doi:10.1021/acs.langmuir.9b02990

data_1557280
_publ_section_title
;
 Regulation of the Metal Center and Coordinating Anion of Mononuclear
 Ln(III) Complexes to Promote an Efficient Luminescence Response to
 Various Organic Solvents
;
_journal_name_full               Langmuir
_journal_paper_doi               10.1021/acs.langmuir.9b02990
_journal_year                    2020
_chemical_formula_moiety         'C25 H26 Dy N9 O6 S, C2 H3 N'
_chemical_formula_sum            'C27 H29 Dy N10 O6 S'
_chemical_formula_weight         784.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.684(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.249(5)
_cell_length_b                   10.064(4)
_cell_length_c                   26.264(11)
_cell_measurement_reflns_used    1048
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.20
_cell_measurement_theta_min      2.55
_cell_volume                     3237(2)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1494
_diffrn_reflns_av_unetI/netI     0.1874
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            17863
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.428
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1564
_refine_diff_density_max         0.773
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5926
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1807
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1972
_reflns_number_gt                2716
_reflns_number_total             5926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            la9b02990_si_002.cif
_cod_data_source_block           aaaa
_cod_database_code               1557280
_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
C19 \\sim C24 \\sim C16 \\sim C23 \\sim C17 \\sim C9 \\sim C8 \\sim C2 \\sim
C18 \\sim C4 \\sim C20 \\sim C25 \\sim C22 \\sim C15 \\sim C7 \\sim C6 \\sim C5
\\sim C10 \\sim C11 \\sim C21 \\sim C3 \\sim C14 \\sim C1 \\sim C27 \\sim C26
\\sim C12 \\sim C13: within 3.8A with sigma of 0.02 and sigma for terminal
atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C15(H15), C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C14(H14A,H14B), C12(H12A,H12B), C13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C23(H23), C9(H9), C4(H4), C20(H20), C22(H22), C6(H6), C5(H5),
 C21(H21), C3(H3)
3.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C1(H1A,H1B,H1C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'