X-ray crystallographic analysis of the antiferromagnetic low-temperature phase of galvinoxyl: investigating magnetic duality in organic radicals.
Suizu, Rie; Shuku, Yoshiaki; Robert, Vincent; Roseiro, Pablo; Ben Amor, Nadia; Khawar, Zain; Robertson, Neil; Awaga, Kunio; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1961–1965; doi:10.1039/d3dt03601d

data_7714695
_publ_section_title
;
 X-ray crystallographic analysis of the antiferromagnetic low-temperature
 phase of galvinoxyl: investigating magnetic duality in organic radicals.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1961
_journal_page_last               1965
_journal_paper_doi               10.1039/d3dt03601d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C29 H41 O2'
_chemical_formula_sum            'C29 H41 O2'
_chemical_formula_weight         421.62
_chemical_name_systematic        Galvinoxyl
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-21 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.837(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5123(3)
_cell_length_b                   10.6991(3)
_cell_length_c                   22.8903(7)
_cell_measurement_reflns_used    7687
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.7950
_cell_measurement_theta_min      3.8070
_cell_volume                     2536.67(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      3.00  29.00   0.50   90.00    --    1.30  45.00 150.00   52
  2  \w     54.00  80.00   0.50   90.00    --    1.30  45.00 120.00   52
  3  \w    -85.00  90.00   0.50   90.00    --    1.30  45.00 176.34  350
  4  \w     25.00  51.00   0.50   90.00    --    2.70  45.00 -12.06   52
  5  \w    -86.00  10.00   0.50   90.00    --    2.70  45.00 -12.06  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0004370000
_diffrn_orient_matrix_UB_12      0.0203179000
_diffrn_orient_matrix_UB_13      -0.0295627000
_diffrn_orient_matrix_UB_21      -0.0026602000
_diffrn_orient_matrix_UB_22      -0.0630419000
_diffrn_orient_matrix_UB_23      -0.0096468000
_diffrn_orient_matrix_UB_31      -0.0684090000
_diffrn_orient_matrix_UB_32      0.0022836000
_diffrn_orient_matrix_UB_33      -0.0048267000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19035
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.129
_diffrn_reflns_theta_min         3.312
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       rod
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0674P)^2^+1.5269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2968
_reflns_number_total             3364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03601d2.cif
_cod_data_source_block           20230208_galvinoxyl_01
_cod_depositor_comments
'Adding full bibliography for 7714695--7714696.cif.'
_cod_database_code               7714695
_shelx_shelxl_version_number     2018/3
_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:
 C4(H4), C5(H5), C7(H7)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              56999
_olex2_submission_special_instructions 'No special instructions were received'