Structural peculiarities and luminescence of europium dipivaloylmethanates with 2,2′-bipyridine derivatives. Polymorphism of [Eu(DPM)3Bpy]
Zhuravlev, Konstantin P.; Tsaryuk, Vera I.; Vologzhanina, Anna V.; Dorovatovskii, Pavel V.; Zubavichus, Yan V.; Kudryashova, Valentina A.; Klemenkova, Zinaida S.; Inorganica Chimica Acta 502 (2020) 119294–; doi:10.1016/j.ica.2019.119294

data_1565472
_publ_section_title
;
 Structural peculiarities and luminescence of europium
 dipivaloylmethanates with 2,2&#x2032;-bipyridine derivatives.
 Polymorphism of [Eu(DPM)3Bpy]
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119294
_journal_paper_doi               10.1016/j.ica.2019.119294
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C43 H65 Eu N2 O6'
_chemical_formula_sum            'C43 H65 Eu N2 O6'
_chemical_formula_weight         857.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                76.96(3)
_cell_angle_beta                 85.79(3)
_cell_angle_gamma                69.96(3)
_cell_formula_units_Z            2
_cell_length_a                   10.990(2)
_cell_length_b                   12.350(3)
_cell_length_c                   17.570(4)
_cell_measurement_reflns_used    150
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.781
_cell_measurement_theta_min      4.002
_cell_volume                     2182.5(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Mar CCD'
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80248
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28882
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        28.783
_diffrn_reflns_theta_max         30.773
_diffrn_reflns_theta_min         3.481
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    2.032
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.839
_refine_diff_density_min         -2.225
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.0209(11)
_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   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         9397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+2.2198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8943
_reflns_number_total             9397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119246.cif
_cod_data_source_block           1
_cod_original_cell_volume        2182.5(9)
_cod_database_code               1565472
_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:
 C13(H13), C24(H24), C34(H34), C45(H45), C41(H41), C40(H40), C39(H39),
 C33(H33), C42(H42), C36(H36), C35(H35)
2.b Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C49(H49A,H49B,H49C), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C21(H21A,
 H21B,H21C), C19(H19A,H19B,H19C), C53(H53A,H53B,H53C), C18(H18A,H18B,H18C),
 C32(H32A,H32B,H32C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C30(H30A,H30B,
 H30C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C16(H16A,H16B,H16C)
;