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_1564039
_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 Gd N14 O6, 2(C6 H6)'
_chemical_formula_sum            'C63 H65 Gd N14 O6'
_chemical_formula_weight         1271.54
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 123.7840(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4959(18)
_cell_length_b                   18.5702(10)
_cell_length_c                   22.5305(12)
_cell_measurement_reflns_used    4068
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     11995.8(11)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_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      120.15
_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  0.0731
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66472
_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         27.999
_diffrn_reflns_theta_min         1.820
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0705 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.7889.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.977
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         14486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0233P)^2^+12.6401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0819
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11180
_reflns_number_total             14486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-513-119922.CIF
_cod_data_source_block           I
_cod_database_code               1564039
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.759
_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:
 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), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S),
 C7S(H7S), C8S(H8S), C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S)
2.b 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)
;