Three new mononuclear tri-spin lanthanide-nitronyl nitroxide radical compounds: syntheses, structures and magnetic properties.
Li, Lei-Lei; Liu, Shuang; Zhang, Yuan; Shi, Wei; Cheng, Peng; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6118–6125; doi:10.1039/c4dt03941f

data_7034055
_publ_section_title
;
 Three new mononuclear tri-spin lanthanide-nitronyl nitroxide radical
 compounds: syntheses, structures and magnetic properties.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6118
_journal_page_last               6125
_journal_paper_doi               10.1039/c4dt03941f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C15 H19 N2 O4'
_chemical_formula_sum            'C15 H19 N2 O4'
_chemical_formula_weight         291.32
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2014-09-24 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                102.611(6)
_cell_angle_beta                 96.527(5)
_cell_angle_gamma                96.021(5)
_cell_formula_units_Z            4
_cell_length_a                   9.5761(6)
_cell_length_b                   10.1949(7)
_cell_length_c                   15.8509(10)
_cell_measurement_reflns_used    4666
_cell_measurement_temperature    130.65(10)
_cell_measurement_theta_max      28.8820
_cell_measurement_theta_min      3.7510
_cell_volume                     1486.87(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.65(10)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -1.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   57.0000 -150.0000 78

  2 omega  -26.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   19.0000  150.0000 109

  3 omega   -6.00   21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   81.0000  147.0000 27

  4 omega   -8.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -99.0000  -60.0000 66

  5 omega  -46.00   29.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -57.0000  -30.0000 75

  6 omega  -35.00   10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1310  -81.0000   24.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0704027000
_diffrn_orient_matrix_UB_12      0.0143439000
_diffrn_orient_matrix_UB_13      0.0030001000
_diffrn_orient_matrix_UB_21      0.0240979000
_diffrn_orient_matrix_UB_22      0.0484752000
_diffrn_orient_matrix_UB_23      0.0398500000
_diffrn_orient_matrix_UB_31      0.0110523000
_diffrn_orient_matrix_UB_32      0.0511847000
_diffrn_orient_matrix_UB_33      -0.0234114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10464
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             620
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.2320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                4333
_reflns_number_total             5240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03941f2.cif
_cod_data_source_block           p140527e
_cod_depositor_comments
'Adding full bibliography for 7034055--7034058.cif.'
_cod_original_cell_volume        1486.88(17)
_cod_database_code               7034055
_chemical_oxdiff_formula         'C H O N'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C24(H24), C28(H28), C9(H9), C13(H13), C27(H27), C25(H25)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C3(H3A,H3B,H3C),
 C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C5(H5A,H5B,H5C), C21(H21A,H21B,H21C),
 C30(H30A,H30B,H30C), C15(H15A,H15B,H15C)
;