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_7714696
_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      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
_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                77.953(9)
_cell_angle_beta                 81.876(11)
_cell_angle_gamma                74.138(11)
_cell_formula_units_Z            4
_cell_length_a                   10.3090(15)
_cell_length_b                   12.8561(13)
_cell_length_c                   20.165(2)
_cell_measurement_reflns_used    2805
_cell_measurement_temperature    50.15
_cell_measurement_theta_max      29.2940
_cell_measurement_theta_min      2.1180
_cell_volume                     2504.1(5)
_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)'
_diffrn_ambient_temperature      50.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.894
_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    -84.00  91.00   0.50   48.00    --    5.00  19.00 120.00  350
  2  \w     42.00  68.00   0.50   48.00    --    5.00  38.00-120.00   52
  3  \w    -64.00  35.00   0.50   48.00    --  -20.40  57.00-180.00  198
  4  \w    -61.00   9.00   0.50   48.00    --  -20.40  76.00  60.00  140
  5  \w    -64.00  11.00   0.50   48.00    --  -20.40  76.00-170.31  150
  6  \w    -63.00  62.00   0.50   48.00    --  -20.40  57.00  30.00  250
  7  \w    -58.00  30.00   0.50   48.00    --  -20.40  76.00 -60.00  176
  8  \w    -31.00  54.00   0.50   48.00    --  -20.40  66.00 -98.45  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0620139000
_diffrn_orient_matrix_UB_12      -0.0406661000
_diffrn_orient_matrix_UB_13      0.0041193000
_diffrn_orient_matrix_UB_21      -0.0210222000
_diffrn_orient_matrix_UB_22      -0.0152601000
_diffrn_orient_matrix_UB_23      0.0348954000
_diffrn_orient_matrix_UB_31      -0.0294945000
_diffrn_orient_matrix_UB_32      -0.0388789000
_diffrn_orient_matrix_UB_33      -0.0083340000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1727
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27511
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.062
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41047
_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_colour_primary    black
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         27511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.2111
_refine_ls_R_factor_gt           0.1160
_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^)+(0.1929P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2909
_refine_ls_wR_factor_ref         0.3362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12146
_reflns_number_total             27511
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9926\% 
 around [-0.00 -0.32 0.95] (reciprocal) or [0.05 -0.73 0.68] (direct)
;
_cod_data_source_file            d3dt03601d2.cif
_cod_data_source_block           20230315_18_50k_2_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7714695--7714696.cif.'
_cod_original_cell_volume        2504.0(6)
_cod_database_code               7714696
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H41O2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5983(19)
 0.4017(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C7A(H7A), C9A(H9A), C10A(H10A), C4B(H4B), C5B(H5B),
 C7B(H7B), C9B(H9B), C10B(H10B)
3.b Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C19A(H19A,
 H19B,H19C), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C), C23A(H23A,H23B,H23C),
 C24A(H24A,H24B,H24C), C25A(H25A,H25B,H25C), C27A(H27A,H27B,H27C), C28A(H28A,
 H28B,H28C), C29A(H29A,H29B,H29C), C01G(H01A,H01B,H01C), C15B(H15D,H15E,H15F),
 C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C19B(H19D,H19E,H19F), C20B(H20D,
 H20E,H20F), C21B(H21D,H21E,H21F), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F),
 C26B(H26A,H26B,H26C), C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F)
;
_shelx_res_checksum              98706
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.007
_oxdiff_exptl_absorpt_empirical_full_min 0.289
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2