First 4,7-oxygenated 1,10-phenanthroline-2,9-diamides: synthesis, tautomerism and complexation with REE nitrates.
Avagyan, Nane A.; Lemport, Pavel S.; Roznyatovsky, Vitaly A.; Averin, Alexei D.; Yakushev, Alexei A.; Lyssenko, Konstantin A.; Perfilyev, Pavel D.; Isakovskaya, Ksenia L.; Aksenova, Svetlana A.; Nelyubina, Yulia V.; Vokuev, Mikhail F.; Rodin, Igor A.; Gloriozov, Igor P.; Ustynyuk, Yuri A.; Nenajdenko, Valentine G.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3052–3064; doi:10.1039/d3dt03643j

data_7714954
_publ_section_title
;
 First 4,7-oxygenated 1,10-phenanthroline-2,9-diamides: synthesis,
 tautomerism and complexation with REE nitrates.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3052
_journal_page_last               3064
_journal_paper_doi               10.1039/d3dt03643j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'(C32 H30 Eu N7 O13), 1.75 (C2 H3 N), 0.25 H2 O'
_chemical_formula_sum            'C35.5 H35.75 Eu N8.75 O13.25'
_chemical_formula_weight         948.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2024-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.6700(16)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   20.2198(5)
_cell_length_b                   31.5715(7)
_cell_length_c                   27.0149(7)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.41
_cell_volume                     16026.7(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon III detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1346
_diffrn_reflns_av_unetI/netI     0.1612
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            118912
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.584
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.641
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6010
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             7664
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.827
_exptl_transmission_factor_min   0.525
_refine_diff_density_max         2.758
_refine_diff_density_min         -1.922
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2109
_refine_ls_number_reflns         36364
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+6.7241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.2076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20031
_reflns_number_total             36364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03643j2.cif
_cod_data_source_block           a_sq
_cod_depositor_comments
'Adding full bibliography for 7714953--7714954.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C35.50 H35.75 Eu N8.75 O13.25'
_cod_database_code               7714954
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.525
_shelx_estimated_absorpt_t_max   0.827
_shelx_res_checksum              30025
_shelx_fab_checksum              48926