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_7131644
_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         'C40 H34 O4, C H2 Cl2'
_chemical_formula_sum            'C41 H36 Cl2 O4'
_chemical_formula_weight         663.60
_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             2021-09-20
_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                90
_cell_angle_beta                 105.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.02420(10)
_cell_length_b                   30.1775(4)
_cell_length_c                   13.9999(2)
_cell_measurement_reflns_used    11742
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.2920
_cell_measurement_theta_min      3.5530
_cell_volume                     3273.46(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 0.999
_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      6.00  82.00   0.80    2.00    --   42.61 -99.00  60.00   95
  2  \w     27.00  97.40   0.80    2.00    --   42.61-125.00 -30.00   88
  3  \w     20.00 116.00   0.80    2.00    --   42.61  37.00-150.00  120
  4  \w     16.00 112.00   0.80    2.00    --   42.61  57.00 -90.00  120
  5  \w    103.00 177.40   0.80    8.00    --  111.00  76.00-154.00   93
  6  \w    104.00 177.60   0.80    8.00    --  111.00 111.00-120.00   92
  7  \w     40.00 134.40   0.80    8.00    --  111.00 -45.00  60.00  118
  8  \w     40.00 134.40   0.80    8.00    --  111.00 -45.00 -60.00  118
  9  \w    103.00 177.40   0.80    8.00    --  111.00  77.00  90.00   93
 10  \w    104.00 177.60   0.80    8.00    --  111.00 111.00 -90.00   92
 11  \w     36.00 108.00   0.80    8.00    --  111.00-111.00 -90.00   90
 12  \w     41.00 138.60   0.80    8.00    --  111.00 -61.00 120.00  122
 13  \w     83.00 177.40   0.80    8.00    --  111.00  61.00-120.00  118
 14  \w     30.00 106.00   0.80    8.00    --  111.00 -94.00 -90.00   95
 15  \w     36.00 108.00   0.80    8.00    --  111.00-111.00 -60.00   90
 16  \w    -65.00  29.40   0.80    2.00    --  -42.61  37.00   0.00  118
 17  \w    -69.00  27.00   0.80    2.00    --  -42.61  57.00-150.00  120
 18  \w     16.00 112.00   0.80    2.00    --   42.61  57.00  90.00  120
 19  \w     16.00 112.00   0.80    2.00    --   42.61  57.00   0.00  120
 20  \w     66.00 152.40   0.80    8.00    --  111.00  15.00  60.00  108
;
_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      0.0712866000
_diffrn_orient_matrix_UB_12      -0.0333927000
_diffrn_orient_matrix_UB_13      -0.0627617000
_diffrn_orient_matrix_UB_21      0.1706493000
_diffrn_orient_matrix_UB_22      0.0261118000
_diffrn_orient_matrix_UB_23      0.0209754000
_diffrn_orient_matrix_UB_31      0.0730140000
_diffrn_orient_matrix_UB_32      -0.0284419000
_diffrn_orient_matrix_UB_33      0.0927669000
_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  0.0167
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16896
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.446
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.127
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.700
_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            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3346
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0651
_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^)+(0.0973P)^2^+4.8628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1836
_refine_ls_wR_factor_ref         0.1853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3173
_reflns_number_total             3346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01301d2.cif
_cod_data_source_block           cavl1709
_cod_depositor_comments
'Adding full bibliography for 7131644--7131646.cif.'
_cod_database_code               7131644
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.618
_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. Restrained distances
 Cl1-C21 \\sim Cl2-C21
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C21 \\sim Cl1 \\sim Cl2: within 3A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 3A
4. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) Cl1(0.5) Cl2(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C12(H12), C13(H13), C20(H20)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              4422
_shelx_hkl_checksum              8333