Proton-assisted seven-electron acceptor properties of di-iso-propylphenyl-bis-iminoacenaphthene.
Khrizanforova, Vera V.; Fayzullin, Robert R.; Morozov, Vladimir I.; Budnikova, Yulia H.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11659–11663; doi:10.1039/d4dt01039f

data_7716475
_publ_section_title
;
 Proton-assisted seven-electron acceptor properties of
 di-iso-propylphenyl-bis-iminoacenaphthene.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11659
_journal_page_last               11663
_journal_paper_doi               10.1039/d4dt01039f
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H63 N2 Na O2'
_chemical_formula_sum            'C44 H63 N2 Na O2'
_chemical_formula_weight         674.95
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-04-02 deposited with the CCDC.	2024-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.9362(2)
_cell_length_b                   11.9362(2)
_cell_length_c                   24.8045(7)
_cell_measurement_reflns_used    37742
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.46
_cell_volume                     3060.51(11)
_computing_cell_refinement       'APEX4 v2021.10-0 (Bruker AXS)'
_computing_data_collection       'APEX4 v2021.10-0 (Bruker AXS)'
_computing_data_reduction        'APEX4 v2021.10-0 (Bruker AXS)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012);
PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      101(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            152341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         2.134
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.9427
_exptl_absorpt_correction_T_min  0.9165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group 3(H) for scaling and error model
 Mean and maximum errors in direction cosine check function =   0.000   0.000
 Restraint esd for equal adjacent scale factors =  0.0100
 Maximum odd and even orders for spherical harmonics =   1   4

 wR2(int) =  0.1649 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0700 (selected reflections only, after parameter refinement)

  156781 total and   9880 unique reflections.
 Reflections rejected for which |I-<I>|/su >   3.00
 where:  su^2 = sigma(I)^2 + (  0.04000 <I>)^2  (sigma(I) from SAINT)

  155284 total and   9877 unique reflections left after |I-<I>|/su test
 su^2 = [K*sigma(I)]^2 + [g<I>]^2  where sigma(I) is from SAINT

 Error model 5: refine all K and overall g
 Run 2theta R(int) Incid. factors Diffr. factors    K      g   I/s(lim) Total I>2sig(I)
   1  24.0  0.0682  0.052 - 0.104  1.019 - 1.039  0.948  0.0263  38.0   12532    9529
   2  24.0  0.0618  0.026 - 0.077  1.018 - 1.039  0.932  0.0263  38.0   16039   12021
   3  24.0  0.0636  0.069 - 0.085  1.018 - 1.039  0.934  0.0263  38.0   11809    9227
   4  24.0  0.0637  0.064 - 0.096  1.018 - 1.039  0.939  0.0263  38.0   11831    9287
   5  24.0  0.0635  0.073 - 0.089  1.019 - 1.039  0.945  0.0263  38.0   11506    9003
   6  24.0  0.0708  0.027 - 0.095  1.018 - 1.039  0.927  0.0263  38.0   26898   20151
   7  24.0  0.0700  0.027 - 0.095  1.018 - 1.039  0.926  0.0263  38.0   26259   19904
   8   0.0  0.0893  0.031 - 0.078  1.020 - 1.038  0.986  0.0263  38.0   13075    9693
   9   0.0  0.0953  0.036 - 0.089  1.018 - 1.039  0.997  0.0263  38.0   12779    9292
  10   0.0  0.0933  0.038 - 0.088  1.018 - 1.039  0.984  0.0263  38.0   12556    9199

  155284 Corrected reflections written to file hkl
 Estimated minimum and maximum transmission:  0.9165  0.9427
 Additional spherical absorption correction applied with mu*r =  0.0100
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 3447 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.13(10)
_refine_ls_extinction_coef       0.0045(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         8622
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0249P)^2^+0.8261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7717
_reflns_number_total             8622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01039f2.cif
_cod_data_source_block           khriz047
_cod_depositor_comments
'Adding full bibliography for 7716473--7716476.cif.'
_cod_original_cell_volume        3060.50(14)
_cod_database_code               7716475
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              89994
_shelx_hkl_checksum              39428