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_7240795
_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 H19 N5 O8 P2'
_chemical_formula_sum            'C11 H19 N5 O8 P2'
_chemical_formula_weight         411.25
_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
_atom_sites_solution_primary     iterative
_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                 103.400(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9985(2)
_cell_length_b                   11.8275(3)
_cell_length_c                   17.5639(3)
_cell_measurement_reflns_used    13095
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.0112
_cell_measurement_theta_min      2.8426
_cell_volume                     1818.43(7)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega -100.00   44.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.2351    0.0000  240.0000 144

  2 omega  -74.00   -3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.2351  100.0000  271.0000 71

  3 omega  -96.00    5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.2351  -77.0000   60.0000 101

  4 omega   57.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.4851  179.0000  270.0000 52

  5 omega  -25.00   24.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.4851  -99.0000  268.0000 49

  6 omega   56.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.4851  179.0000   90.0000 53

  7 omega -101.00    5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.2351  -77.0000  180.0000 106

  8 omega -101.00    5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.2351  -77.0000  270.0000 106

  9 omega  -24.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       29.4851 -100.0000   88.0000 99
;
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0390291796
_diffrn_orient_matrix_UB_12      0.0044565309
_diffrn_orient_matrix_UB_13      0.0306344881
_diffrn_orient_matrix_UB_21      0.0658171781
_diffrn_orient_matrix_UB_22      0.0246835784
_diffrn_orient_matrix_UB_23      0.0245530211
_diffrn_orient_matrix_UB_31      -0.0265806854
_diffrn_orient_matrix_UB_32      0.0544358651
_diffrn_orient_matrix_UB_33      -0.0136079684
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30070
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.895
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
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    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5285
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0737P)^2^+0.4322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3911
_reflns_number_total             5285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04714g2.cif
_cod_data_source_block           kiev96
_cod_depositor_comments
'Adding full bibliography for 7240795--7240798.cif.'
_cod_database_code               7240795
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.893
_reflns_odcompleteness_completeness 93.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.03
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1-O1A
 1.58 with sigma of 0.001
 P1-O1B
 1.58 with sigma of 0.001
 O1A-C1A
 1.43 with sigma of 0.001
 O1B-C1B
 1.43 with sigma of 0.001
 P1-O2A
 1.58 with sigma of 0.001
 P1-O2B
 1.58 with sigma of 0.001
 O2A-C2A
 1.43 with sigma of 0.001
 O2B-C2B
 1.43 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
O2A \\sim C2A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1A \\sim C1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O2B \\sim C2B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1B \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: O1A(0.7) O2A(0.7) C1A(0.7) H1AA(0.7) H1AB(0.7) H1AC(0.7) C2A(0.7)
 H2AA(0.7) H2AB(0.7) H2AC(0.7) O1B(0.3) O2B(0.3) C1B(0.3) H1BA(0.3) H1BB(0.3)
 H1BC(0.3) C2B(0.3) H2BA(0.3) H2BB(0.3) H2BC(0.3)
5.a Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C1B(H1BA,H1BB,H1BC), C2B(H2BA,H2BB,H2BC)
;
_olex2_submission_special_instructions 'No special instructions were received'