Synthesis, crystal structure and photophysical properties of mixed-ligand lanthanide complexes with 1,3-diketonates bearing pyrazole moieties and 1,10-phenanthroline
Taydakov, Ilya V.; Korshunov, Vladislav M.; Belousov, Yuriy A.; Nelyubina, Yulia V.; Marchetti, Fabio; Pettinari, Riccardo; Pettinari, Claudio; Inorganica Chimica Acta 513 (2020) 119922–; doi:10.1016/j.ica.2020.119922

data_1564040
_publ_section_title
;
 Synthesis, crystal structure and photophysical properties of mixed-ligand
 lanthanide complexes with 1,3-diketonates bearing pyrazole moieties and
 1,10-phenanthroline
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119922
_journal_paper_doi               10.1016/j.ica.2020.119922
_journal_volume                  513
_journal_year                    2020
_chemical_formula_moiety
'C51 H53 N14 O6 Yb, 1.75(C H2 Cl2), C7 H8, 0.75(H2 O)'
_chemical_formula_sum            'C59.75 H66 Cl3.5 N14 O6.75 Yb'
_chemical_formula_weight         1385.38
_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   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 97.8510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2382(9)
_cell_length_b                   20.2285(15)
_cell_length_c                   25.7802(19)
_cell_measurement_reflns_used    6664
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     6322.3(8)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            78446
_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         25.999
_diffrn_reflns_theta_min         1.758
_exptl_absorpt_coefficient_mu    1.689
_exptl_absorpt_correction_T_max  0.2657
_exptl_absorpt_correction_T_min  0.1947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0866 before and 0.0646 after correction.
The Ratio of minimum to maximum transmission is 0.7328.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.729
_refine_diff_density_min         -2.556
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00053(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         12422
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+40.9966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9292
_reflns_number_total             12422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-513-119922.CIF
_cod_data_source_block           II
_cod_original_formula_sum        'C59.75 H66 Cl3.50 N14 O6.75 Yb'
_cod_database_code               1564040
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.677
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3S-Cl5S \\sim C3S-Cl6S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C7S) \\sim Ueq, Uanis(C6S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C3S) = Uanis(C2S)
Uanis(Cl5S) = Uanis(Cl3S)
Uanis(Cl4S) = Uanis(Cl6S)
4. Others
 Fixed Sof: C1S(0.75) H1SA(0.75) H1SB(0.75) Cl1S(0.75) Cl2S(0.75) C2S(0.75)
 H2SA(0.75) H2SB(0.75) Cl3S(0.75) Cl4S(0.75) O1W(0.75) H1WA(0.75) H1WB(0.75)
 Cl6S(0.25) Cl5S(0.25) C3S(0.25) H3SA(0.25) H3SB(0.25)
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11),
 C15(H15), C20(H20), C11A(H11A), C15A(H15A), C20A(H20A), C11B(H11B), C15B(H15B),
  C20B(H20B), C4S(H4S), C5S(H5S), C6S(H6S), C7S(H7S), C8S(H8S)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F), C22A(H22D,H22E,H22F),
 C23A(H23D,H23E,H23F), C17B(H17G,H17H,H17I), C18B(H18G,H18H,H18I), C22B(H22G,
 H22H,H22I), C23B(H23G,H23H,H23I), C9S(H9SA,H9SB,H9SC)
;