Coexistence of long-range antiferromagnetic order and slow relaxation of the magnetization in the first lanthanide complex of a 1,2,4-benzotriazinyl radical
Morgan, Ian; Mansikkamäki, Akseli; Rouzieres, Mathieu; Clerac, Rodolphe; Tuononen, Heikki M.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02766D

data_7044201
_publ_section_title
;
 Coexistence of long-range antiferromagnetic order and slow relaxation of
 the magnetization in the first lanthanide complex of a
 1,2,4-benzotriazinyl radical
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02766D
_journal_year                    2017
_chemical_formula_moiety         'C51 H70 Dy N4 O6'
_chemical_formula_sum            'C51 H70 Dy N4 O6'
_chemical_formula_weight         997.61
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.640(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3358(2)
_cell_length_b                   23.0105(7)
_cell_length_c                   21.1555(6)
_cell_measurement_reflns_used    5005
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.1630
_cell_measurement_theta_min      4.3480
_cell_volume                     5031.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -34.00   18.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4926   37.0000 -180.0000 52

  2 omega  -85.00   -9.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4926  125.0000    0.0000 76

  3 omega   23.00   63.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4926 -125.0000  -90.0000 40

  4 omega  -25.00   41.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4926  -57.0000  -60.0000 66

  5 omega   84.00  176.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   61.0000  -60.0000 92

  6 omega   30.00  109.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -94.0000 -180.0000 79

  7 omega  111.00  152.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -30.0000 41

  8 omega   39.00   99.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 60

  9 omega   44.00  150.00   1.0000  130.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -15.0000  -90.0000 106
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0824594000
_diffrn_orient_matrix_UB_12      0.0513270000
_diffrn_orient_matrix_UB_13      -0.0242090000
_diffrn_orient_matrix_UB_21      0.0097626000
_diffrn_orient_matrix_UB_22      0.0287779000
_diffrn_orient_matrix_UB_23      0.0656096000
_diffrn_orient_matrix_UB_31      0.1237825000
_diffrn_orient_matrix_UB_32      0.0319716000
_diffrn_orient_matrix_UB_33      -0.0202620000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16869
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.987
_diffrn_reflns_theta_min         4.180
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.336
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       plate
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.0761
_exptl_crystal_size_mid          0.0502
_exptl_crystal_size_min          0.0175
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         9300
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0302P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6923
_reflns_number_total             9300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02766d2.cif
_cod_data_source_block           im02-35-dytbacac3pybl_red
_cod_database_code               7044201
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C51 H70 O6 N4 Dy1'
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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. Restrained distances
 C4B-C1B = C4B-C3BB
 1.5 with sigma of 0.05
 C3A-C4A = C4A-C2AA = C4A-C2AA = C3A-C4A
 1.5 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
C3A \\sim C3A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C2AA \\sim C2AA: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C1C \\sim C1CC: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C3A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C2AA)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3BB) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.008
Uanis(C1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3C) \\sim Ueq, Uanis(C3C) \\sim Ueq, Uanis(C1CC) \\sim Ueq, Uanis(C1C)
\\sim Ueq, Uanis(C2CC) \\sim Ueq, Uanis(C2CC) \\sim Ueq: with sigma of 0.005
and sigma for terminal atoms of 0.008
Uanis(C2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2C) \\sim Ueq, Uanis(C3CC) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C2AA)=Sof(H2Aa)=Sof(H2Ab)=Sof(H2Ac)=Sof(C3AA)=Sof(H3Ad)=Sof(H3Ae)=
 Sof(H3Af)=1-FVAR(1)
 Sof(C3A)=Sof(H3Aa)=Sof(H3Ab)=Sof(H3Ac)=Sof(C2A)=Sof(H2Ad)=Sof(H2Ae)=Sof(H2Af)=
 FVAR(1)
 Sof(C3C)=Sof(H3Ca)=Sof(H3Cb)=Sof(H3Cc)=Sof(C2C)=Sof(H2Cd)=Sof(H2Ce)=Sof(H2Cf)=
 Sof(C1C)=Sof(H1Cd)=Sof(H1Ce)=Sof(H1Cf)=1-FVAR(2)
 Sof(C1CC)=Sof(H1Ca)=Sof(H1Cb)=Sof(H1Cc)=Sof(C2CC)=Sof(H2Ca)=Sof(H2Cb)=
 Sof(H2Cc)=Sof(C3CC)=Sof(H3Cd)=Sof(H3Ce)=Sof(H3Cf)=FVAR(2)
 Sof(C2B)=Sof(H2Bd)=Sof(H2Be)=Sof(H2Bf)=Sof(C1B)=Sof(H1Bd)=Sof(H1Be)=Sof(H1Bf)=
 Sof(C3BB)=Sof(H3Bd)=Sof(H3Be)=Sof(H3Bf)=1-FVAR(3)
 Sof(C3B)=Sof(H3Ba)=Sof(H3Bb)=Sof(H3Bc)=Sof(C2BB)=Sof(H2Ba)=Sof(H2Bb)=
 Sof(H2Bc)=Sof(C1BB)=Sof(H1Ba)=Sof(H1Bb)=Sof(H1Bc)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C21(H21), C6C(H6C), C16(H16), C19(H19), C20(H20), C7(H7), C9(H9),
 C8(H8), C6A(H6A), C6(H6), C13(H13), C12(H12), C18(H18), C6B(H6B), C15(H15)
5.b Idealised Me refined as rotating group:
 C1A(H1Aa,H1Ab,H1Ac), C10C(H10a,H10b,H10c), C11C(H11a,H11b,H11c), C11B(H11d,
 H11e,H11f), C9C(H9Ca,H9Cb,H9Cc), C3B(H3Ba,H3Bb,H3Bc), C2AA(H2Aa,H2Ab,H2Ac),
 C10B(H10d,H10e,H10f), C2BB(H2Ba,H2Bb,H2Bc), C9A(H9Aa,H9Ab,H9Ac), C3A(H3Aa,H3Ab,
 H3Ac), C10A(H10g,H10h,H10i), C9B(H9Ba,H9Bb,H9Bc), C1BB(H1Ba,H1Bb,H1Bc),
 C3C(H3Ca,H3Cb,H3Cc), C1CC(H1Ca,H1Cb,H1Cc), C2CC(H2Ca,H2Cb,H2Cc), C11A(H11g,
 H11h,H11i), C2C(H2Cd,H2Ce,H2Cf), C2A(H2Ad,H2Ae,H2Af), C3AA(H3Ad,H3Ae,H3Af),
 C1C(H1Cd,H1Ce,H1Cf), C3CC(H3Cd,H3Ce,H3Cf), C2B(H2Bd,H2Be,H2Bf), C1B(H1Bd,H1Be,
 H1Bf), C3BB(H3Bd,H3Be,H3Bf)
;
_olex2_submission_special_instructions 'No special instructions were received'