Lanthanide complexes based on a new bis-chelating carbacylamidophosphate (CAPh) scorpionate-like ligand
Olyshevets, Iryna; Ovchynnikov, Vladimir; Kariaka, Nataliia; Dyakonenko, Viktoriya; Shishkina, Svitlana; Sliva, Tatiana; Ostrowska, Małgorzata; Jedyńczuk, Aleksandra; Gumienna-Kontecka, Elżbieta; Amirkhanov, Vladimir; RSC Advances 10 (2020) 24808–24816; doi:10.1039/D0RA04714G

data_7240796
_publ_section_title
;
 Lanthanide complexes based on a new bis-chelating carbacylamidophosphate
 (CAPh) scorpionate-like ligand
;
_journal_issue                   42
_journal_name_full               'RSC Advances'
_journal_page_first              24808
_journal_page_last               24816
_journal_paper_doi               10.1039/D0RA04714G
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C22 H36 Eu N11 O19 P4, C3 H8 O'
_chemical_formula_sum            'C25 H44 Eu N11 O20 P4'
_chemical_formula_weight         1094.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-28 deposited with the CCDC.	2020-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.525(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3844(6)
_cell_length_b                   17.2947(6)
_cell_length_c                   19.5123(8)
_cell_measurement_reflns_used    3024
_cell_measurement_temperature    294
_cell_measurement_theta_max      23.4000
_cell_measurement_theta_min      3.2750
_cell_volume                     4330.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  69.00   1.00   20.00    --   27.65 -99.00 150.00   91
  2  \w      0.00  98.00   1.00   20.00    --   27.65  77.00 -30.00   98
  3  \w     39.00  68.00   1.00   20.00    --   27.65 -99.00   0.00   29
  4  \w    -35.00  55.00   1.00   20.00    --   27.65 -77.00-150.00   90
  5  \w    -28.00  10.00   1.00   20.00    --   27.65 -77.00  60.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0408235000
_diffrn_orient_matrix_UB_12      -0.0123603000
_diffrn_orient_matrix_UB_13      0.0139595000
_diffrn_orient_matrix_UB_21      0.0362512000
_diffrn_orient_matrix_UB_22      -0.0215584000
_diffrn_orient_matrix_UB_23      0.0267467000
_diffrn_orient_matrix_UB_31      0.0085473000
_diffrn_orient_matrix_UB_32      0.0326323000
_diffrn_orient_matrix_UB_33      0.0229791000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25701
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       block
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.450
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8470
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0728P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5974
_reflns_number_total             8470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04714g2.cif
_cod_data_source_block           kiev327
_cod_depositor_comments
'Adding full bibliography for 7240795--7240798.cif.'
_cod_original_cell_volume        4330.2(3)
_cod_database_code               7240796
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.632
_shelx_estimated_absorpt_t_min   0.432
_reflns_odcompleteness_completeness 87.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.79
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C24-C23 = C25-C23
 1.45 with sigma of 0.002
 O9-C12 = O10-C13 = O14-C21 = O15-C22 = O7-C11 = O6-C10 = O1-C1 = O2-C2
 1.43 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
O20 \\sim C23 \\sim C24 \\sim C25: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Riding coordinates:
 O20(H20)
4.b Ternary CH refined with riding coordinates:
 C23(H23)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N4(H4), N7(H7), N9(H9), N10(H10), C5(H5), C6(H6), C7(H7A),
 C16(H16), C17(H17), C18(H18)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.711