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_1565477
_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 N2 O6 Tb'
_chemical_formula_sum            'C43 H65 N2 O6 Tb'
_chemical_formula_weight         864.89
_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                   28.015(3)
_cell_length_b                   24.423(3)
_cell_length_c                   12.9837(14)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      2.30
_cell_volume                     8883.6(17)
_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      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1551
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            155430
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         30.145
_diffrn_reflns_theta_min         1.106
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.636
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         3.424
_refine_diff_density_min         -2.295
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
 Flack x determined using 7321 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         26150
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0100P)^2^+50.1223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                19329
_reflns_number_total             26150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119246.cif
_cod_data_source_block           3c
_cod_original_cell_volume        8883.5(16)
_cod_database_code               1565477
_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. Uiso/Uaniso restraints and constraints
C75 \\sim C34A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C74A \\sim C35A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C73 \\sim C33A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C85 \\sim C19A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C21A \\sim C86: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C84A \\sim C20A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C54 \\sim C23A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C56 \\sim C22A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C24A \\sim C55: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C43A) \\sim Ueq, Uanis(C42A) \\sim Ueq, Uanis(C41A) \\sim Ueq: with sigma
of 0.007 and sigma for terminal atoms of 0.014
3. Others
 Fixed Sof: C21A(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C24A(0.5) H24A(0.5)
 H24B(0.5) H24C(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C56(0.5) H56A(0.5)
 H56B(0.5) H56C(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5) C74A(0.5) H74A(0.5)
 H74B(0.5) H74C(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5) C84A(0.5) H84A(0.5)
 H84B(0.5) H84C(0.5) C85(0.5) H85A(0.5) H85B(0.5) H85C(0.5) C19A(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5) C20A(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C22A(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) C23A(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C33A(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34A(0.5) H34A(0.5) H34B(0.5)
 H34C(0.5) C35A(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 H55C(0.5) C86(0.5) H86A(0.5) H86B(0.5) H86C(0.5)
 Fixed Uiso: C21A(0.07)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16),
 C27(H27), C38(H38), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C8A(H8A),
  C9A(H9A), C10A(H10A), C16A(H16A), C27A(H27A), C38A(H38A)
4.b Idealised Me refined as rotating group:
 C11(H11D,H11E,H11F), C12(H12D,H12E,H12F), C13(H13D,H13E,H13F), C19(H19D,H19E,
 H19F), C20(H20D,H20E,H20F), C21(H21D,H21E,H21F), C22(H22D,H22E,H22F), C23(H23D,
 H23E,H23F), C24(H24D,H24E,H24F), C30(H30D,H30E,H30F), C31(H31D,H31E,H31F),
 C32(H32D,H32E,H32F), C33(H33D,H33E,H33F), C34(H34D,H34E,H34F), C35(H35D,H35E,
 H35F), C41(H41D,H41E,H41F), C42(H42D,H42E,H42F), C43(H43D,H43E,H43F),
 C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C30A(H30A,
 H30B,H30C), C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C41A(H41A,H41B,H41C),
 C42A(H42A,H42B,H42C), C43A(H43A,H43B,H43C), C21A(H21A,H21B,H21C), C24A(H24A,
 H24B,H24C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C73(H73A,H73B,H73C),
 C74A(H74A,H74B,H74C), C75(H75A,H75B,H75C), C84A(H84A,H84B,H84C), C85(H85A,H85B,
 H85C), C19A(H19A,H19B,H19C), C20A(H20A,H20B,H20C), C22A(H22A,H22B,H22C),
 C23A(H23A,H23B,H23C), C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C35A(H35A,
 H35B,H35C), C55(H55A,H55B,H55C), C86(H86A,H86B,H86C)
;