Verdazyl Radical, a Building Block for a Six-Spin-Center 2p-3d-4f Single-Molecule Magnet.
Novitchi, Ghénadie; Shova, Sergiu; Lan, Yanhua; Wernsdorfer, Wolfgang; Train, Cyrille; Inorganic chemistry 55 (2016) 12122–12125; doi:10.1021/acs.inorgchem.6b02380

data_4349319
_publ_section_title
;
 Verdazyl Radical, a Building Block for a Six-Spin-Center 2p-3d-4f
 Single-Molecule Magnet.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12122
_journal_page_last               12125
_journal_paper_doi               10.1021/acs.inorgchem.6b02380
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C18 H23 Co Dy N5 O10'
_chemical_formula_sum            'C18 H23 Co Dy N5 O10'
_chemical_formula_weight         690.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                108.594(11)
_cell_angle_beta                 94.039(9)
_cell_angle_gamma                117.126(15)
_cell_formula_units_Z            2
_cell_length_a                   10.2001(13)
_cell_length_b                   10.6945(18)
_cell_length_c                   13.1719(12)
_cell_measurement_reflns_used    1254
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      23.8820
_cell_measurement_theta_min      1.6780
_cell_volume                     1171.7(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.05(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega   -6.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5127   76.0000  -33.0000 89

  2 omega  -46.00   49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5127  -76.0000 -159.0000 95

  3 omega   -4.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0127   38.0000   90.0000 59

  4 omega  -25.00   18.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0127  -99.0000   90.0000 43

  5 omega   35.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5127  178.0000  150.0000 58

  6 omega   55.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5127   57.0000  120.0000 32
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0047345000
_diffrn_orient_matrix_UB_12      0.0702472000
_diffrn_orient_matrix_UB_13      0.0056294000
_diffrn_orient_matrix_UB_21      -0.0269310000
_diffrn_orient_matrix_UB_22      0.0033742000
_diffrn_orient_matrix_UB_23      0.0484512000
_diffrn_orient_matrix_UB_31      0.0760571000
_diffrn_orient_matrix_UB_32      0.0404475000
_diffrn_orient_matrix_UB_33      0.0327845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.2228
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7829
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.687
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.935
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61455
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.615
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4132
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2448
_reflns_number_total             4132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02380_si_002.cif
_cod_data_source_block           exp_2633
_cod_original_cell_volume        1171.7(3)
_cod_database_code               4349319
_chemical_oxdiff_formula         'C15 H20 N3 O4 Co1 Dy1'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'