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_1565476
_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 Gd N2 O6'
_chemical_formula_sum            'C43 H65 Gd N2 O6'
_chemical_formula_weight         863.22
_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                   28.065(2)
_cell_length_b                   24.460(2)
_cell_length_c                   13.0005(11)
_cell_measurement_reflns_used    5221
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.21
_cell_volume                     8924.5(12)
_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  0.1876
_diffrn_reflns_av_unetI/netI     0.1827
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            110762
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         30.659
_diffrn_reflns_theta_min         1.104
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.2657
_exptl_absorpt_correction_T_min  0.1993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0985 before and 0.0850 after correction.
The Ratio of minimum to maximum transmission is 0.7501.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.298
_refine_diff_density_min         -2.757
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Flack x determined using 4718 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.028(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         27490
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1669
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+40.1494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1643
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                14748
_reflns_number_total             27490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119246.cif
_cod_data_source_block           3b
_cod_original_cell_volume        8924.5(13)
_cod_database_code               1565476
_olex2_refinement_description
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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
C35A \\sim C75A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C33A \\sim C74: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C34A \\sim C73: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C20A \\sim C85A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C19A \\sim C86: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C21A \\sim C84: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C65A \\sim C42A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C43A \\sim C66A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C41A \\sim C67: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C23) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of
0.006 and sigma for terminal atoms of 0.012
Uanis(C23A) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma
of 0.007 and sigma for terminal atoms of 0.014
Uanis(C11) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(C30) = Uanis(C9)
3. Others
 Fixed Sof: C19A(0.5) H19D(0.5) H19E(0.5) H19F(0.5) C20A(0.5) H20D(0.5)
 H20E(0.5) H20F(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C33A(0.5)
 H33D(0.5) H33E(0.5) H33F(0.5) C34A(0.5) H34D(0.5) H34E(0.5) H34F(0.5)
 C35A(0.5) H35D(0.5) H35E(0.5) H35F(0.5) C41A(0.5) H41D(0.5) H41E(0.5)
 H41F(0.5) C43A(0.5) H43D(0.5) H43E(0.5) H43F(0.5) C65A(0.5) H65A(0.5)
 H65B(0.5) H65C(0.5) C42A(0.5) H42D(0.5) H42E(0.5) H42F(0.5) C66A(0.5)
 H66A(0.5) H66B(0.5) H66C(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) H73C(0.5) C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5) C75A(0.5)
 H75A(0.5) H75B(0.5) H75C(0.5) C84(0.5) H84A(0.5) H84B(0.5) H84C(0.5) C85A(0.5)
 H85A(0.5) H85B(0.5) H85C(0.5) C86(0.5) H86A(0.5) H86B(0.5) H86C(0.5)
 Fixed Uiso: C19A(0.07)
4.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C8A(H8A), C9A(H9A),
 C10A(H10A), C16A(H16A), C27A(H27A), C38A(H38A), C1(H10), C2(H9), C3(H8),
 C4(H7), C7(H4), C8(H3), C9(H2), C10(H1), C16(H38), C27(H16), C38(H27)
4.b Idealised Me refined as rotating group:
 C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C22A(H22D,
 H22E,H22F), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C30A(H30D,H30E,H30F),
 C31A(H31D,H31E,H31F), C32A(H32D,H32E,H32F), C19A(H19D,H19E,H19F), C20A(H20D,
 H20E,H20F), C21A(H21D,H21E,H21F), C33A(H33D,H33E,H33F), C34A(H34D,H34E,H34F),
 C35A(H35D,H35E,H35F), C41A(H41D,H41E,H41F), C43A(H43D,H43E,H43F), C65A(H65A,
 H65B,H65C), C42A(H42D,H42E,H42F), C66A(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75A(H75A,H75B,H75C), C84(H84A,H84B,
 H84C), C85A(H85A,H85B,H85C), C86(H86A,H86B,H86C), C11(H43A,H43B,H43C),
 C12(H41A,H41B,H41C), C13(H42A,H42B,H42C), C19(H34A,H34B,H34C), C20(H33A,H33B,
 H33C), C21(H35A,H35B,H35C), C22(H19A,H19B,H19C), C23(H20A,H20B,H20C), C24(H21A,
 H21B,H21C), C30(H13A,H13B,H13C), C31(H12A,H12B,H12C), C32(H11A,H11B,H11C),
 C33(H32A,H32B,H32C), C34(H31A,H31B,H31C), C35(H30A,H30B,H30C), C40(H23A,H23B,
 H23C), C41(H24A,H24B,H24C), C42(H22A,H22B,H22C)
;