Effects of the Dzyaloshinskii-Moriya interaction in Cr3 triangular spin clusters detected by specific heat and multi-frequency electron spin resonance.
Ghirri, Alberto; van Tol, Johan; Vitorica-Yrezabal, Inigo; Timco, Grigore A.; Winpenny, Richard E. P.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14027–14033; doi:10.1039/c5dt01938a

data_7035621
_publ_section_title
;
 Effects of the Dzyaloshinskii-Moriya interaction in Cr3 triangular spin
 clusters detected by specific heat and multi-frequency electron spin
 resonance.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14027
_journal_page_last               14033
_journal_paper_doi               10.1039/c5dt01938a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C30 H60 Cr3 O16, 2(C5 H9 O2), 2(C2 H5 O)'
_chemical_formula_sum            'C44 H91 Cr3 O22'
_chemical_formula_weight         1128.17
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-15 deposited with the CCDC.
2015-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.2920(6)
_cell_length_b                   12.2920(6)
_cell_length_c                   22.7190(13)
_cell_measurement_reflns_used    2319
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      26.3430
_cell_measurement_theta_min      3.7670
_cell_volume                     2972.8(3)
_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, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details
;
  1 omega  -57.00  -31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.1866   19.0000 -120.0000 26

  2 omega  -53.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.6554    0.0000 -180.0000 114
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0327788000
_diffrn_orient_matrix_UB_12      0.0291943000
_diffrn_orient_matrix_UB_13      0.0114912000
_diffrn_orient_matrix_UB_21      0.0195718000
_diffrn_orient_matrix_UB_22      0.0413314000
_diffrn_orient_matrix_UB_23      -0.0244520000
_diffrn_orient_matrix_UB_31      -0.0546092000
_diffrn_orient_matrix_UB_32      -0.0432986000
_diffrn_orient_matrix_UB_33      -0.0156540000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7877
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.168
_diffrn_reflns_theta_min         3.301
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53671
_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 bluish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1428
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1142P)^2^+2.8421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1089
_reflns_number_total             1428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01938a1.cif
_cod_data_source_block           arepw512
_cod_depositor_comments          'Adding full bibliography for 7035621.cif.'
_cod_database_code               7035621
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         cR7nI1n3o32f8c200h200
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C16-C15
 2.4 with sigma of 0.02
 C15-C17
 2.4 with sigma of 0.02
 C17-C16
 2.4 with sigma of 0.02
 C13-C14
 1.54 with sigma of 0.02
 C16-C14
 1.54 with sigma of 0.02
 C14-C17
 1.54 with sigma of 0.02
 C14-C15
 1.54 with sigma of 0.02
 C16-C13
 2.4 with sigma of 0.02
 C17-C14
 1.54 with sigma of 0.02
 C17-C13
 2.4 with sigma of 0.02
 C15-C14
 1.54 with sigma of 0.02
 C15-C13
 2.4 with sigma of 0.02
 C14-C17
 1.54 with sigma of 0.02
 C22-C23
 1.54 with sigma of 0.02
 O12-O11
 2.2 with sigma of 0.02
 O11-C13
 1.3 with sigma of 0.02
 C13-O12
 1.3 with sigma of 0.02
 O11-C15
 2.9 with sigma of 0.02
 C16-O11
 2.9 with sigma of 0.02
 O11-C14
 2.35 with sigma of 0.02
 O12-C14
 2.35 with sigma of 0.02
 C23-O21
 2.4 with sigma of 0.02
 O21-C22
 1.3 with sigma of 0.002
 C23-O21
 2.4 with sigma of 0.02
3. Restrained planarity
 C14, C13, O12, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O21 \\sim O11 \\sim O12: within 1.7A with sigma of 0.002 and sigma for terminal
atoms of 0.004
5. Rigid body (RIGU) restrains
 C14, C16, C13, C15, C17, O12, O11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O21, C22, C23
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C5, C4, C6, C3, C2, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 H4C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) H41A(0.25) H41B(0.25) C14(0.16667)
 O12(0.16667) C13(0.16667) O21(0.16667) C22(0.16667) H22A(0.16667)
 H22B(0.16667) C23(0.16667) H23A(0.16667) H23B(0.16667) H23C(0.16667)
 O11(0.16667) C16(0.16667) H16A(0.16667) H16B(0.16667) H16C(0.16667)
 C15(0.16667) H15A(0.16667) H15B(0.16667) H15C(0.16667) C17(0.16667)
 H17A(0.16667) H17B(0.16667) H17C(0.16667)
7.a Rotating group:
 O41(H41A,H41B)
7.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
7.c Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C23(H23A,H23B,H23C),
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              18345
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_date_sample_data_collection 2014-03-18
_olex2_submission_special_instructions 'No special instructions were received'