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_7240797
_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 N11 O19 P4 Tb, C3 H8 O'
_chemical_formula_sum            'C25 H44 N11 O20 P4 Tb'
_chemical_formula_weight         1101.51
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-16 deposited with the CCDC.	2020-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.506(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.134(2)
_cell_length_b                   17.152(2)
_cell_length_c                   19.453(3)
_cell_measurement_reflns_used    934
_cell_measurement_temperature    110
_cell_measurement_theta_max      18.6650
_cell_measurement_theta_min      3.2450
_cell_volume                     4179.3(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    9.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645   57.0000  150.0000 85

  2 omega   -9.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -99.0000 -120.0000 78

  3 omega   26.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -99.0000   30.0000 43

  4 omega  -38.00   11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -57.0000  -90.0000 49

  5 omega   12.00   38.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -57.0000  -90.0000 26

  6 omega  -14.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -57.0000  -60.0000 58

  7 omega   36.00   61.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645 -178.0000   60.0000 25

  8 omega   27.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -77.0000  120.0000 30

  9 omega   -4.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645   19.0000   90.0000 103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0192364000
_diffrn_orient_matrix_UB_12      0.0071071000
_diffrn_orient_matrix_UB_13      -0.0375927000
_diffrn_orient_matrix_UB_21      -0.0442989000
_diffrn_orient_matrix_UB_22      -0.0246795000
_diffrn_orient_matrix_UB_23      -0.0024423000
_diffrn_orient_matrix_UB_31      -0.0294480000
_diffrn_orient_matrix_UB_32      0.0324787000
_diffrn_orient_matrix_UB_33      0.0063158000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1810
_diffrn_reflns_av_unetI/netI     0.1656
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33047
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.935
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.858
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0753P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.2067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4081
_reflns_number_total             7352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04714g2.cif
_cod_data_source_block           kiev301_lt
_cod_depositor_comments
'Adding full bibliography for 7240795--7240798.cif.'
_cod_original_cell_volume        4179.6(12)
_cod_database_code               7240797
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.445
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: -1(10)
 2(10)
2. 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
3. Restrained distances
 O10-C13B
 1.45 with sigma of 0.002
 O10-C13A
 1.45 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C13B) = Uanis(C13A)
Uanis(C25) = Uanis(C24)
5. Others
 Fixed Sof: C13A(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C13B(0.5) H13D(0.5)
 H13E(0.5) H13F(0.5)
6.a Ternary CH refined with riding coordinates:
 C23(H23)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N5(H5), N7(H7), N9(H9), N10(H10), C5(H5A), C6(H6), C7(H7A),
 C16(H16), C17(H17), C18(H18)
6.c 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), C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
6.d Idealised tetrahedral OH refined as rotating group:
 O20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'