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_7240798
_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         'C11 H18 N5 Na O8 P2, C3 H8 O'
_chemical_formula_sum            'C14 H26 N5 Na O9 P2'
_chemical_formula_weight         493.33
_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   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                 108.507(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.740(2)
_cell_length_b                   17.912(3)
_cell_length_c                   9.9299(15)
_cell_measurement_reflns_used    837
_cell_measurement_temperature    294
_cell_measurement_theta_max      18.8020
_cell_measurement_theta_min      3.3830
_cell_volume                     2317.5(7)
_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      294
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1827
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -23.00    3.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.3583  -77.0000  150.0000 26

  2 omega    0.00   77.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645   77.0000  120.0000 77

  3 omega  -42.00   14.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -57.0000   60.0000 56

  4 omega   23.00   69.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645  -99.0000    0.0000 46

  5 omega   19.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645   57.0000 -150.0000 77

  6 omega  -12.00   70.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645   19.0000   60.0000 82

  7 omega    6.00   89.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       26.7645   57.0000  -60.0000 83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0366633000
_diffrn_orient_matrix_UB_12      -0.0292764000
_diffrn_orient_matrix_UB_13      0.0156133000
_diffrn_orient_matrix_UB_21      0.0186185000
_diffrn_orient_matrix_UB_22      0.0127180000
_diffrn_orient_matrix_UB_23      -0.0548944000
_diffrn_orient_matrix_UB_31      0.0356096000
_diffrn_orient_matrix_UB_32      0.0234820000
_diffrn_orient_matrix_UB_33      0.0491756000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1295
_diffrn_reflns_av_unetI/netI     0.1453
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20367
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.127
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34264
_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    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.2012
_refine_ls_R_factor_gt           0.0964
_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^)+(0.0667P)^2^+1.1471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.2182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2506
_reflns_number_total             5320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04714g2.cif
_cod_data_source_block           k300a
_cod_depositor_comments
'Adding full bibliography for 7240795--7240798.cif.'
_cod_original_cell_volume        2317.5(6)
_cod_database_code               7240798
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.881
_reflns_odcompleteness_completeness 89.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.35
_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. Uiso/Uaniso restraints and constraints
O9 \\sim C12 \\sim C13 \\sim C14: within 1.8A with sigma of 0.005 and sigma for
terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C12(H12)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N5(H5), C5(H5A), C6(H6), C7(H7)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
3.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'