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_1565475
_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_absolute_configuration ad
_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      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.021(6)
_cell_length_b                   24.455(5)
_cell_length_c                   13.015(3)
_cell_measurement_reflns_used    329
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.682
_cell_measurement_theta_min      4.021
_cell_volume                     8919(3)
_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
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0656
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69853
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        28.783
_diffrn_reflns_theta_max         30.874
_diffrn_reflns_theta_min         3.265
_exptl_absorpt_coefficient_mu    1.990
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       prism
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.752
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 7222 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.460(5)
_refine_ls_extinction_coef       0.0036(2)
_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   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         18210
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.003
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+7.0738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1219
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    0.862
_reflns_Friedel_fraction_max     0.865
_reflns_number_gt                17253
_reflns_number_total             18210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119246.cif
_cod_data_source_block           3a
_cod_original_cell_volume        8918(3)
_cod_database_code               1565475
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.658
_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. Restrained distances
 C2A-C67
 1.5 with sigma of 0.02
 C03U-C67
 1.5 with sigma of 0.02
 C3A-C84 = C03R-C83 = C03D-C82
 1.5 with sigma of 0.02
 C03R-C78 = C3A-C78 = C84-C78 = C83-C78
 1.5 with sigma of 0.02
 C2A-C03U
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C2A) = Uiso(C69) = Uiso(C03U) = Uiso(C70) = Uiso(C025) = Uiso(C68)
4. Others
 Fixed Sof: C025(0.5) H02A(0.5) H02B(0.5) H02C(0.5) C69(0.5) H69A(0.5)
 H69B(0.5) H69C(0.5) C70(0.5) H70A(0.5) H70B(0.5) H70C(0.5) C82(0.5) H82A(0.5)
 H82B(0.5) H82C(0.5) C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5) C84(0.5) H84A(0.5)
 H84B(0.5) H84C(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C03D(0.5) H03A(0.5)
 H03B(0.5) H03C(0.5) C03R(0.5) H03D(0.5) H03E(0.5) H03F(0.5) C03U(0.5)
 H03G(0.5) H03H(0.5) H03I(0.5) C68(0.5) H68A(0.5) H68B(0.5) H68C(0.5) C2A(0.5)
 H2AA(0.5) H2AB(0.5) H2AC(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C23(H23),
 C34(H34), C45(H45), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18),
  C19(H19), C20(H20), C56(H56), C66(H66), C76(H76)
5.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C01H(H01A,H01B,H01C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C72(H72A,
 H72B,H72C), C73(H73A,H73B,H73C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C),
 C81(H81A,H81B,H81C), C025(H02A,H02B,H02C), C69(H69A,H69B,H69C), C70(H70A,H70B,
 H70C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C3A(H3AA,
 H3AB,H3AC), C03D(H03A,H03B,H03C), C03R(H03D,H03E,H03F), C03U(H03G,H03H,H03I),
 C68(H68A,H68B,H68C), C2A(H2AA,H2AB,H2AC)
;