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_1565473
_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 Eu N2 O6'
_chemical_formula_sum            'C45 H69 Eu N2 O6'
_chemical_formula_weight         885.98
_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                74.240(2)
_cell_angle_beta                 80.046(2)
_cell_angle_gamma                68.276(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2423(4)
_cell_length_b                   12.3046(4)
_cell_length_c                   19.0305(6)
_cell_measurement_reflns_used    9569
_cell_measurement_temperature    120
_cell_measurement_theta_max      71.77
_cell_measurement_theta_min      3.97
_cell_volume                     2345.91(14)
_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      120.0
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8869
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.311
_diffrn_reflns_theta_min         2.420
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.912
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1542 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.5009.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.240
_refine_diff_density_min         -2.648
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+49.9576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2066
_refine_ls_wR_factor_ref         0.2097
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8191
_reflns_number_total             8869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119246.cif
_cod_data_source_block           2
_cod_database_code               1565473
_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(0.031) H43(0.027) H34(0.033) H40(0.023) H45A(0.043)
 H45B(0.043) H45C(0.043) H42(0.026) H6(0.029) H32A(0.056) H32B(0.056)
 H32C(0.056) H35(0.039) H37(0.03) H28(0.03) H10A(0.056) H10B(0.056) H10C(0.056)
 H9A(0.053) H9B(0.053) H9C(0.053) H12A(0.057) H12B(0.057) H12C(0.057)
 H33A(0.057) H33B(0.057) H33C(0.057) H31A(0.067) H31B(0.067) H31C(0.067)
 H13A(0.062) H13B(0.062) H13C(0.062) H14A(0.07) H14B(0.07) H14C(0.07)
 H22A(0.062) H22B(0.062) H22C(0.062) H11A(0.062) H11B(0.062) H11C(0.062)
 H44A(0.056) H44B(0.056) H44C(0.056) H20A(0.077) H20B(0.077) H20C(0.077)
 H21A(0.069) H21B(0.069) H21C(0.069) H1A(0.063) H1B(0.063) H1C(0.063)
 H2A(0.054) H2B(0.054) H2C(0.054) H23A(0.087) H23B(0.087) H23C(0.087)
 H3A(0.074) H3B(0.074) H3C(0.074) H24A(0.094) H24B(0.094) H24C(0.094)
 H25A(0.089) H25B(0.089) H25C(0.089) H3AA(0.08) H3AB(0.08) H3AC(0.08)
 H1AA(0.037) H1AB(0.037) H1AC(0.037) H2AA(0.081) H2AB(0.081) H2AC(0.081)
 H23D(0.087) H23E(0.087) H23F(0.087) H25D(0.089) H25E(0.089) H25F(0.089)
 H24D(0.094) H24E(0.094) H24F(0.094)
 Fixed X: H17(1.066) H43(1.2194) H34(0.7992) H40(0.8189) H45A(0.9308)
 H45B(1.0591) H45C(0.9252) H42(1.1947) H6(1.3274) H32A(1.418) H32B(1.54)
 H32C(1.4513) H35(0.5847) H37(0.6692) H28(1.1322) H10A(1.531) H10B(1.6155)
 H10C(1.4825) H9A(1.4069) H9B(1.5333) H9C(1.3948) H12A(1.2539) H12B(1.3688)
 H12C(1.2258) H33A(1.4064) H33B(1.5111) H33C(1.3732) H31A(1.3207) H31B(1.4594)
 H31C(1.3327) H13A(1.4135) H13B(1.4886) H13C(1.3693) H14A(1.3106) H14B(1.4506)
 H14C(1.3915) H22A(0.8851) H22B(0.737) H22C(0.8468) H11A(1.4918) H11B(1.621)
 H11C(1.5409) H44A(0.4173) H44B(0.4554) H44C(0.4279) H20A(0.8045) H20B(0.7195)
 H20C(0.8712) H21A(0.7331) H21B(0.6336) H21C(0.7039) H1A(0.9378) H1B(0.9248)
 H1C(0.9118) H2A(1.0096) H2B(1.0636) H2C(1.1598) H23A(0.9305) H23B(0.8382)
 H23C(0.9874) H3A(1.2762) H3B(1.1604) H3C(1.2103) H24A(0.9791) H24B(0.8267)
 H24C(0.9082) H25A(0.7438) H25B(0.6894) H25C(0.7576) H3AA(1.2609) H3AB(1.1258)
 H3AC(1.183) H1AA(0.9805) H1AB(0.9527) H1AC(0.9095) H2AA(1.1042) H2AB(1.0993)
 H2AC(1.2309) H23D(0.9062) H23E(0.8059) H23F(0.9568) H25D(0.7649) H25E(0.6894)
 H25F(0.7791) H24D(0.9586) H24E(0.8131) H24F(0.8434)
 Fixed Y: H17(0.8314) H43(0.5332) H34(0.3786) H40(0.6728) H45A(0.8277)
 H45B(0.7359) H45C(0.7143) H42(0.6364) H6(0.0353) H32A(0.3516) H32B(0.2337)
 H32C(0.3017) H35(0.4419) H37(0.6387) H28(0.2405) H10A(0.2017) H10B(0.2211)
 H10C(0.3236) H9A(0.3269) H9B(0.2207) H9C(0.2094) H12A(0.8311) H12B(0.8403)
 H12C(0.8807) H33A(0.1089) H33B(0.0488) H33C(0.0333) H31A(0.1126) H31B(0.125)
 H31C(0.2387) H13A(0.5237) H13B(0.6161) H13C(0.6221) H14A(0.7316) H14B(0.6979)
 H14C(0.5947) H22A(0.9553) H22B(0.9739) H22C(0.8661) H11A(0.0084) H11B(0.0353)
 H11C(0.0046) H44A(0.661) H44B(0.6258) H44C(0.5308) H20A(0.8502) H20B(0.9675)
 H20C(0.9375) H21A(0.7264) H21B(0.8484) H21C(0.739) H1A(0.0666) H1B(0.0036)
 H1C(0.1424) H2A(0.1041) H2B(-0.0396) H2C(0.0342) H23A(0.4492) H23B(0.3817)
 H23C(0.3086) H3A(-0.1016) H3B(-0.1523) H3C(-0.0969) H24A(0.1931) H24B(0.224)
 H24C(0.1608) H25A(0.3394) H25B(0.4214) H25C(0.4692) H3AA(-0.1251) H3AB(-
 0.1366) H3AC(-0.0521) H1AA(0.07) H1AB(-0.0238) H1AC(0.1153) H2AA(0.065) H2AB(-
 0.0662) H2AC(-0.04) H23D(0.4917) H23E(0.4428) H23F(0.3708) H25D(0.4728)
 H25E(0.4451) H25F(0.525) H24D(0.1627) H24E(0.2207) H24F(0.1962)
 Fixed Z: H17(0.1518) H43(0.3509) H34(0.2781) H40(0.4687) H45A(0.4967)
 H45B(0.5335) H45C(0.561) H42(0.4406) H6(0.3609) H32A(0.0402) H32B(0.0627)
 H32C(0.1239) H35(0.3234) H37(0.4329) H28(0.0546) H10A(0.2543) H10B(0.3063)
 H10C(0.2823) H9A(0.4102) H9B(0.4407) H9C(0.4685) H12A(0.0623) H12B(0.097)
 H12C(0.1351) H33A(0.1971) H33B(0.1377) H33C(0.1516) H31A(0.0278) H31B(0.0029)
 H31C(-0.0179) H13A(0.1367) H13B(0.1008) H13C(0.0628) H14A(0.2539) H14B(0.2114)
 H14C(0.2515) H22A(0.0929) H22B(0.0909) H22C(0.061) H11A(0.4318) H11B(0.3971)
 H11C(0.3481) H44A(0.3723) H44B(0.4548) H44C(0.4226) H20A(0.2803) H20B(0.2265)
 H20C(0.2238) H21A(0.1524) H21B(0.172) H21C(0.2357) H1A(0.4112) H1B(0.3509)
 H1C(0.329) H2A(0.239) H2B(0.2559) H2C(0.2245) H23A(-0.0202) H23B(-0.0287)
 H23C(-0.0185) H3A(0.3356) H3B(0.3656) H3C(0.4168) H24A(0.0365) H24B(0.0455)
 H24C(0.1157) H25A(0.163) H25B(0.0866) H25C(0.1329) H3AA(0.3802) H3AB(0.4172)
 H3AC(0.4413) H1AA(0.4281) H1AB(0.3949) H1AC(0.3541) H2AA(0.2297) H2AB(0.2689)
 H2AC(0.2608) H23D(0.0001) H23E(-0.0201) H23F(-0.0292) H25D(0.1364)
 H25E(0.0832) H25F(0.0499) H24D(0.0853) H24E(0.0636) H24F(0.1468)
;