Dimethylnonacethrene - <i>en route</i> to a magnetic switch.
Čavlović, Daniel; Blacque, Olivier; Krummenacher, Ivo; Braunschweig, Holger; Ravat, Prince; Juríček, Michal; Chemical communications (Cambridge, England) 59 (2023) 7743–7746; doi:10.1039/d3cc01301d

data_7131645
_publ_section_title
;
 Dimethylnonacethrene - <i>en route</i> to a magnetic switch.
;
_journal_issue                   50
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7743
_journal_page_last               7746
_journal_paper_doi               10.1039/d3cc01301d
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C38 H26 O2'
_chemical_formula_sum            'C38 H26 O2'
_chemical_formula_weight         514.59
_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     dual
_audit_creation_date             2021-09-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-01-02 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                71.820(3)
_cell_angle_beta                 73.113(3)
_cell_angle_gamma                74.791(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1425(3)
_cell_length_b                   12.3731(4)
_cell_length_c                   13.4276(5)
_cell_measurement_reflns_used    13872
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.3500
_cell_measurement_theta_min      3.5360
_cell_volume                     1207.72(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -87.00  -6.00   1.00    2.00    --  -42.61 125.00-120.00   81
  2  \w   -116.00 -20.00   1.00    2.00    --  -42.61 -37.00 -60.00   96
  3  \w   -113.00 -16.00   1.00    2.00    --  -42.61 -57.00  60.00   97
  4  \w    -69.00  28.00   1.00    2.00    --  -42.61  57.00-150.00   97
  5  \w     11.00  42.00   1.00    2.00    --   42.61  79.00  65.49   31
  6  \w     30.00 107.00   1.00    8.00    --  111.00 -94.00 150.00   77
  7  \w    104.00 178.00   1.00    8.00    --  111.00 111.00-180.00   74
  8  \w     37.00 142.00   1.00    8.00    --  111.00 -77.00-120.00  105
  9  \w     36.00 109.00   1.00    8.00    --  111.00-111.00-120.00   73
 10  \w     83.00 178.00   1.00    8.00    --  111.00  61.00 -60.00   95
 11  \w     36.00 109.00   1.00    8.00    --  111.00-111.00  60.00   73
 12  \w     83.00 178.00   1.00    8.00    --  111.00  61.00 -30.00   95
 13  \w     87.00 178.00   1.00    8.00    --  111.00  30.00 -90.00   91
 14  \w     36.00 109.00   1.00    8.00    --  111.00-111.00   0.00   73
 15  \w     30.00 107.00   1.00    8.00    --  111.00 -94.00-180.00   77
 16  \w    103.00 178.00   1.00    8.00    --  111.00  77.00 -90.00   75
 17  \w     40.00 135.00   1.00    8.00    --  111.00 -45.00 150.00   95
 18  \w     81.00 178.00   1.00    8.00    --  111.00  71.00  -3.08   97
 19  \w     36.00 109.00   1.00    8.00    --  111.00-111.00 -60.00   73
 20  \w     36.00 109.00   1.00    8.00    --  111.00-111.00 150.00   73
 21  \w     61.00 146.00   1.00    8.00    --  111.00 178.00 120.00   85
 22  \w     36.00 109.00   1.00    8.00    --  111.00-111.00 -90.00   73
 23  \w    103.00 178.00   1.00    8.00    --  111.00  77.00-150.00   75
 24  \w    103.00 178.00   1.00    8.00    --  111.00  77.00 120.00   75
 25  \w     41.00 123.00   1.00    8.00    --  111.00-138.00 156.59   82
 26  \w   -113.00 -16.00   1.00    2.00    --  -42.61 -57.00-150.00   97
 27  \w    -87.00  -6.00   1.00    2.00    --  -42.61 125.00   0.00   81
 28  \w   -116.00 -20.00   1.00    2.00    --  -42.61 -37.00 120.00   96
 29  \w     11.00  42.00   1.00    2.00    --   42.61  76.00 -20.79   31
 30  \w     10.00  42.00   1.00    2.00    --   42.61  82.00 168.44   32
 31  \w     88.00 178.00   1.00    8.00    --  111.00  39.00-166.27   90
 32  \w     83.00 178.00   1.00    8.00    --  111.00  62.00  81.54   95
 33  \w     87.00 178.00   1.00    8.00    --  111.00  30.00  90.00   91
 34  \w     83.00 178.00   1.00    8.00    --  111.00  61.00 150.00   95
 35  \w     83.00 178.00   1.00    8.00    --  111.00  61.00-150.00   95
 36  \w     84.00 178.00   1.00    8.00    --  111.00  59.00  36.37   94
 37  \w     83.00 178.00   1.00    8.00    --  111.00  61.00 -90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1489215000
_diffrn_orient_matrix_UB_12      0.0568772000
_diffrn_orient_matrix_UB_13      -0.0597052000
_diffrn_orient_matrix_UB_21      0.1251977000
_diffrn_orient_matrix_UB_22      0.0683407000
_diffrn_orient_matrix_UB_23      -0.0933176000
_diffrn_orient_matrix_UB_31      0.0518592000
_diffrn_orient_matrix_UB_32      -0.0995210000
_diffrn_orient_matrix_UB_33      -0.0557347000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23349
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.493
_diffrn_reflns_theta_min         3.558
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
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)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0427
_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^+0.3678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4341
_reflns_number_total             4924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01301d2.cif
_cod_data_source_block           cavl1609
_cod_depositor_comments
'Adding full bibliography for 7131644--7131646.cif.'
_cod_database_code               7131645
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.872
_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.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C35(H35A,H35B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C10(H10), C12(H12), C13(H13), C19(H19), C20(H20), C25(H25),
 C26(H26), C29(H29), C30(H30), C34(H34)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              63676
_shelx_hkl_checksum              42896