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_1565474
_publ_section_title
;
 Structural peculiarities and luminescence of europium
 dipivaloylmethanates with 2,2&#x2032;-bipyridine derivatives.
 Polymorphism of [Eu(DPM)3Bpy]
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_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         'C45 H69 N2 O6 Tb'
_chemical_formula_sum            'C45 H69 N2 O6 Tb'
_chemical_formula_weight         892.94
_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                74.311(4)
_cell_angle_beta                 79.747(4)
_cell_angle_gamma                68.215(3)
_cell_formula_units_Z            2
_cell_length_a                   11.272(2)
_cell_length_b                   12.305(2)
_cell_length_c                   19.043(4)
_cell_measurement_reflns_used    5283
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.23
_cell_volume                     2352.4(8)
_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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1453
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14880
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         31.266
_diffrn_reflns_theta_min         1.115
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.547
_exptl_absorpt_correction_T_max  0.2657
_exptl_absorpt_correction_T_min  0.1670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1187 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.6285.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       prism
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.909
_refine_diff_density_min         -4.379
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         14880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+18.4439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1964
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10645
_reflns_number_total             14880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119246.cif
_cod_data_source_block           2a
_cod_original_cell_volume        2352.2(7)
_cod_database_code               1565474
_olex2_refinement_description
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1. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C3(0.5) H3A(0.5) H3B(0.5)
 H3C(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) H3AC(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5)
 H1AC(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) C23A(0.5) H23D(0.5) H23E(0.5)
 H23F(0.5) C25A(0.5) H25D(0.5) H25E(0.5) H25F(0.5) C24A(0.5) H24D(0.5)
 H24E(0.5) H24F(0.5)
 Fixed Uiso: H17(0.03) H43(0.025) H34(0.031) H40(0.027) H45A(0.044)
 H45B(0.044) H45C(0.044) H42(0.026) H6(0.032) H32A(0.051) H32B(0.051)
 H32C(0.051) H35(0.037) H37(0.031) H28(0.031) H10A(0.048) H10B(0.048)
 H10C(0.048) H9A(0.056) H9B(0.056) H9C(0.056) H12A(0.054) H12B(0.054)
 H12C(0.054) H33A(0.057) H33B(0.057) H33C(0.057) H31A(0.062) H31B(0.062)
 H31C(0.062) H13A(0.057) H13B(0.057) H13C(0.057) H14A(0.067) H14B(0.067)
 H14C(0.067) H22A(0.06) H22B(0.06) H22C(0.06) H11A(0.061) H11B(0.061)
 H11C(0.061) H44A(0.055) H44B(0.055) H44C(0.055) H20A(0.083) H20B(0.083)
 H20C(0.083) H21A(0.072) H21B(0.072) H21C(0.072) H1A(0.055) H1B(0.055)
 H1C(0.055) H2A(0.057) H2B(0.057) H2C(0.057) H23A(0.095) H23B(0.095)
 H23C(0.095) H3A(0.067) H3B(0.067) H3C(0.067) H24A(0.092) H24B(0.092)
 H24C(0.092) H25A(0.082) H25B(0.082) H25C(0.082) H3AA(0.067) H3AB(0.067)
 H3AC(0.067) H1AA(0.055) H1AB(0.055) H1AC(0.055) H2AA(0.057) H2AB(0.057)
 H2AC(0.057) H23D(0.095) H23E(0.095) H23F(0.095) H25D(0.082) H25E(0.082)
 H25F(0.082) H24D(0.092) H24E(0.092) H24F(0.092)
 Fixed X: H17(1.0627) H43(1.2221) H34(0.8007) H40(0.818) H45A(0.9253)
 H45B(1.0593) H45C(0.9316) H42(1.1942) H6(1.3259) H32A(1.4216) H32B(1.541)
 H32C(1.448) H35(0.5879) H37(0.6723) H28(1.1332) H10A(1.53) H10B(1.6141)
 H10C(1.4811) H9A(1.3943) H9B(1.5289) H9C(1.3987) H12A(1.2441) H12B(1.3713)
 H12C(1.2362) H33A(1.4223) H33B(1.5077) H33C(1.3654) H31A(1.324) H31B(1.4599)
 H31C(1.3302) H13A(1.42) H13B(1.4852) H13C(1.3659) H14A(1.3124) H14B(1.4523)
 H14C(1.3892) H22A(0.8929) H22B(0.7415) H22C(0.8391) H11A(1.4828) H11B(1.6146)
 H11C(1.5393) H44A(0.4184) H44B(0.4592) H44C(0.4288) H20A(0.8033) H20B(0.7156)
 H20C(0.8667) H21A(0.7275) H21B(0.6322) H21C(0.7149) H1A(0.9397) H1B(0.923)
 H1C(0.9081) H2A(1.0145) H2B(1.0407) H2C(1.1568) H23A(0.9281) H23B(0.8442)
 H23C(0.9934) H3A(1.2739) H3B(1.1569) H3C(1.2114) H24A(0.9681) H24B(0.8154)
 H24C(0.9006) H25A(0.7408) H25B(0.69) H25C(0.7539) H3AA(1.2608) H3AB(1.128)
 H3AC(1.1678) H1AA(0.9888) H1AB(0.9351) H1AC(0.9176) H2AA(1.0756) H2AB(1.1091)
 H2AC(1.2193) H23D(0.8938) H23E(0.8192) H23F(0.9723) H25D(0.7491) H25E(0.7018)
 H25F(0.8074) H24D(0.8689) H24E(0.7368) H24F(0.8508)
 Fixed Y: H17(0.8309) H43(0.5309) H34(0.3741) H40(0.6724) H45A(0.8262)
 H45B(0.7408) H45C(0.7098) H42(0.6372) H6(0.0366) H32A(0.3493) H32B(0.2313)
 H32C(0.3032) H35(0.4374) H37(0.6379) H28(0.2366) H10A(0.2017) H10B(0.2214)
 H10C(0.3235) H9A(0.3259) H9B(0.2297) H9C(0.2034) H12A(0.8339) H12B(0.8336)
 H12C(0.8782) H33A(0.1091) H33B(0.0404) H33C(0.0378) H31A(0.1089) H31B(0.1267)
 H31C(0.2369) H13A(0.5216) H13B(0.6196) H13C(0.6137) H14A(0.7294) H14B(0.6916)
 H14C(0.5915) H22A(0.9458) H22B(0.9782) H22C(0.867) H11A(0.0082) H11B(0.0331)
 H11C(0.0078) H44A(0.6626) H44B(0.6222) H44C(0.531) H20A(0.8462) H20B(0.9637)
 H20C(0.9366) H21A(0.7352) H21B(0.8448) H21C(0.7239) H1A(0.0747) H1B(0.002)
 H1C(0.1408) H2A(0.1152) H2B(-0.0263) H2C(0.0234) H23A(0.4349) H23B(0.3544)
 H23C(0.2921) H3A(-0.107) H3B(-0.1546) H3C(-0.0976) H24A(0.1826) H24B(0.22)
 H24C(0.1661) H25A(0.3564) H25B(0.4218) H25C(0.4841) H3AA(-0.1184) H3AB(-
 0.1411) H3AC(-0.0526) H1AA(0.034) H1AB(-0.0075) H1AC(0.131) H2AA(0.0624) H2AB(-
 0.0763) H2AC(-0.0175) H23D(0.4966) H23E(0.4245) H23F(0.372) H25D(0.478)
 H25E(0.4731) H25F(0.5337) H24D(0.1784) H24E(0.2815) H24F(0.2392)
 Fixed Z: H17(0.1513) H43(0.3514) H34(0.2804) H40(0.4668) H45A(0.4988)
 H45B(0.5309) H45C(0.563) H42(0.4384) H6(0.3609) H32A(0.0405) H32B(0.0664)
 H32C(0.1251) H35(0.326) H37(0.4334) H28(0.0568) H10A(0.2546) H10B(0.3063)
 H10C(0.2829) H9A(0.4121) H9B(0.4378) H9C(0.4702) H12A(0.066) H12B(0.0925)
 H12C(0.1389) H33A(0.1963) H33B(0.1344) H33C(0.16) H31A(0.0297) H31B(0.0033)
 H31C(-0.016) H13A(0.1384) H13B(0.0963) H13C(0.0646) H14A(0.2541) H14B(0.2118)
 H14C(0.2523) H22A(0.093) H22B(0.0935) H22C(0.0611) H11A(0.4282) H11B(0.399)
 H11C(0.3449) H44A(0.3745) H44B(0.4564) H44C(0.4222) H20A(0.2821) H20B(0.23)
 H20C(0.226) H21A(0.1456) H21B(0.1802) H21C(0.2321) H1A(0.4135) H1B(0.36)
 H1C(0.3308) H2A(0.2366) H2B(0.2567) H2C(0.2251) H23A(-0.023) H23B(-0.0224)
 H23C(-0.0097) H3A(0.3358) H3B(0.3694) H3C(0.4172) H24A(0.0476) H24B(0.0609)
 H24C(0.1292) H25A(0.1627) H25B(0.0835) H25C(0.1223) H3AA(0.3833) H3AB(0.413)
 H3AC(0.4446) H1AA(0.4355) H1AB(0.3787) H1AC(0.3677) H2AA(0.232) H2AB(0.2722)
 H2AC(0.2513) H23D(-0.0029) H23E(-0.0252) H23F(-0.0265) H25D(0.1321)
 H25E(0.059) H25F(0.0538) H24D(0.113) H24E(0.1288) H24F(0.1804)
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