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_7131646
_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         'C66 H66, 2(C6 H6)'
_chemical_formula_sum            'C78 H78'
_chemical_formula_weight         1015.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2023-01-02 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.0918(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.35075(14)
_cell_length_b                   9.98785(8)
_cell_length_c                   16.08593(13)
_cell_measurement_reflns_used    32330
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.3160
_cell_measurement_theta_min      2.3880
_cell_volume                     2947.77(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 1.000
_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   -115.00 -20.50   0.90    2.50    --  -42.36 -37.00  30.00  105
  2  \w    -87.00  -6.00   0.90    2.50    --  -42.36 125.00-150.00   90
  3  \w    -87.00  -6.00   0.90    2.50    --  -42.36 125.00  30.00   90
  4  \w    -65.00  30.40   0.90    2.50    --  -42.36  37.00-150.00  106
  5  \w     20.00 114.50   0.90    2.50    --   42.36  37.00 -60.00  105
  6  \w     27.00  96.30   0.90    2.50    --   42.36-125.00-120.00   77
  7  \w     24.00 177.00   0.90   10.00    --  111.00   0.00  90.00  170
  8  \w     87.00 177.00   0.90   10.00    --  111.00  45.00 120.00  100
  9  \w     41.00 138.20   0.90   10.00    --  111.00 -61.00-180.00  108
 10  \w    103.00 177.70   0.90   10.00    --  111.00  77.00 -90.00   83
 11  \w     87.00 177.00   0.90   10.00    --  111.00  45.00-120.00  100
 12  \w     36.00 108.00   0.90   10.00    --  111.00-111.00  60.00   80
 13  \w     87.00 177.00   0.90   10.00    --  111.00  45.00 -60.00  100
 14  \w     36.00 108.00   0.90   10.00    --  111.00-111.00  90.00   80
 15  \w     61.00 144.70   0.90   10.00    --  111.00 178.00 -90.00   93
 16  \w     36.00 108.00   0.90   10.00    --  111.00-111.00 150.00   80
 17  \w     36.00 108.00   0.90   10.00    --  111.00-111.00 120.00   80
 18  \w     83.00 177.50   0.90   10.00    --  111.00  61.00 -60.00  105
 19  \w     83.00 177.50   0.90   10.00    --  111.00  61.00 150.00  105
 20  \w     30.00 106.50   0.90   10.00    --  111.00 -94.00-180.00   85
 21  \w     87.00 177.00   0.90   10.00    --  111.00  45.00  90.00  100
 22  \w    104.00 177.80   0.90   10.00    --  111.00 111.00-150.00   82
 23  \w     83.00 177.50   0.90   10.00    --  111.00  61.00 120.00  105
 24  \w     30.00 106.50   0.90   10.00    --  111.00 -94.00 150.00   85
 25  \w     40.00 134.50   0.90   10.00    --  111.00 -45.00-120.00  105
 26  \w     87.00 177.00   0.90   10.00    --  111.00  45.00-180.00  100
 27  \w    104.00 177.80   0.90   10.00    --  111.00 111.00-120.00   82
 28  \w     87.00 177.00   0.90   10.00    --  111.00  45.00 -90.00  100
 29  \w    104.00 177.80   0.90   10.00    --  111.00 111.00-180.00   82
 30  \w   -113.00 -16.70   0.90    2.50    --  -42.36 -57.00-150.00  107
 31  \w    -87.00  -6.00   0.90    2.50    --  -42.36 125.00 -60.00   90
 32  \w   -113.00 -16.70   0.90    2.50    --  -42.36 -57.00 150.00  107
 33  \w     16.00 112.30   0.90    2.50    --   42.36  57.00-180.00  107
 34  \w     16.00 112.30   0.90    2.50    --   42.36  57.00  90.00  107
 35  \w     16.00 112.30   0.90    2.50    --   42.36  57.00   0.00  107
 36  \w     83.00 177.50   0.90   10.00    --  111.00  61.00   0.00  105
 37  \w     83.00 129.80   0.90   10.00    --  111.00  61.00  30.00   52
 38  \w     30.00 106.50   0.90   10.00    --  111.00 -94.00 -90.00   85
;
_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      -0.0791070000
_diffrn_orient_matrix_UB_12      0.0455785000
_diffrn_orient_matrix_UB_13      0.0136066000
_diffrn_orient_matrix_UB_21      -0.0137327000
_diffrn_orient_matrix_UB_22      -0.1261892000
_diffrn_orient_matrix_UB_23      0.0525990000
_diffrn_orient_matrix_UB_31      0.0247133000
_diffrn_orient_matrix_UB_32      0.0761544000
_diffrn_orient_matrix_UB_33      0.0788116000
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54916
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.484
_diffrn_reflns_theta_min         2.408
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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            yellow
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;

;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         11491
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0865
_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^)+(0.1886P)^2^+0.7207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2150
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.918
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                10780
_reflns_number_total             11491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01301d2.cif
_cod_data_source_block           cavl0911
_cod_depositor_comments
'Adding full bibliography for 7131644--7131646.cif.'
_cod_database_code               7131646
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.914
_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:
 C14(H14A,H14B), C44(H44A,H44B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C8(H8), C16(H16), C17(H17), C19(H19), C20(H20),
 C23(H23), C25(H25), C27(H27), C37(H37), C38(H38), C46(H46), C47(H47), C49(H49),
  C50(H50), C53(H53), C55(H55), C57(H57), C67(H67), C68(H68), C69(H69),
 C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C58(H58A,
 H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              36675
_shelx_hkl_checksum              76627