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_7716476
_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_formula_moiety
'C88 H114 N4 Na6 O4, 0.278(C6 H14), 1.722(C4 H8 O)'
_chemical_formula_sum            'C96.56 H131.67 N4 Na6 O5.72'
_chemical_formula_weight         1577.90
_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   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                67.9803(13)
_cell_angle_beta                 73.9588(14)
_cell_angle_gamma                80.1701(14)
_cell_formula_units_Z            1
_cell_length_a                   12.7513(7)
_cell_length_b                   12.7725(7)
_cell_length_c                   15.0009(8)
_cell_measurement_reflns_used    55030
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.31
_cell_volume                     2170.5(2)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0643
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            194541
_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         27.103
_diffrn_reflns_theta_min         1.856
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.9357
_exptl_absorpt_correction_T_min  0.8794
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group -1 for scaling and error model
 Mean and maximum errors in direction cosine check function =   0.001   0.005
 Restraint esd for equal adjacent scale factors =  0.0060
 Maximum odd and even orders for spherical harmonics =   1   4

 wR2(int) =  0.1419 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0696 (selected reflections only, after parameter refinement)

  198180 total and  10245 unique reflections assuming Friedel's law
 plus   8753 total and  2553 unique reflections in fast scans
 Reflections rejected for which |I-<I>|/su >   3.00
 where:  su^2 = sigma(I)^2 + (  0.04000 <I>)^2  (sigma(I) from SAINT)

  196470 total and  10242 unique reflections left after |I-<I>|/su test
 plus   8522 total and  2543 unique reflections in fast scans
 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  26.1  0.0596  0.044 - 0.052  1.012 - 1.063  0.878  0.0445  22.4   10069    6864
   2  26.1  0.0590  0.052 - 0.074  1.012 - 1.056  0.889  0.0445  22.4    9743    6520
   3  26.1  0.0623  0.043 - 0.088  1.012 - 1.055  0.874  0.0445  22.4    9755    6471
   4  26.1  0.0620  0.048 - 0.089  1.012 - 1.060  0.895  0.0445  22.4    9467    6352
   5  26.1  0.0639  0.045 - 0.082  1.015 - 1.055  0.909  0.0445  22.4    9692    6389
   6  26.1  0.0605  0.035 - 0.069  1.012 - 1.053  0.875  0.0445  22.4   10368    6946
   7  26.1  0.0716  0.046 - 0.068  1.012 - 1.064  0.937  0.0445  22.4   10318    6723
   8  26.1  0.0624  0.040 - 0.060  1.012 - 1.059  0.907  0.0445  22.4   10695    7080
   9  28.9  0.0664  0.040 - 0.084  1.012 - 1.054  0.862  0.0445  22.4    9448    6291
  10  26.1  0.0679  0.051 - 0.085  1.012 - 1.059  0.878  0.0445  22.4    9763    6491
  11  26.1  0.0616  0.045 - 0.090  1.014 - 1.055  0.847  0.0445  22.4    9094    6199
  12  26.1  0.0623  0.046 - 0.082  1.012 - 1.063  0.888  0.0445  22.4    9771    6550
  13 -26.1  0.0594  0.046 - 0.057  1.012 - 1.057  0.898  0.0445  22.4   10235    6866
  14  26.1  0.0677  0.036 - 0.081  1.012 - 1.065  0.886  0.0445  22.4   16185   10941
  15  26.1  0.0654  0.036 - 0.089  1.012 - 1.056  0.901  0.0445  22.4   17629   11857
  16   0.0  0.0740  0.045 - 0.088  1.012 - 1.061  1.010  0.0445  22.4   11232    7568
  17   0.0  0.0695  0.044 - 0.091  1.012 - 1.059  0.966  0.0445  22.4   11521    7878
  18   0.0  0.0705  0.045 - 0.092  1.012 - 1.059  0.970  0.0445  22.4   11485    7847
  19f  0.0  0.1390  0.419 - 0.884  1.012 - 1.052  0.990  0.0445  22.4    4717    2570
  20f  0.0  0.1318  0.402 - 0.896  1.012 - 1.044  1.025  0.0445  22.4    3805    2156

       0 Overloads replaced by fast scan measurements
  196470 Corrected reflections written to file hkl
 Estimated minimum and maximum transmission:  0.8794  0.9357
 Additional spherical absorption correction applied with mu*r =  0.0100
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       plank
_exptl_crystal_F_000             851
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         9575
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.8690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7811
_reflns_number_total             9575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01039f2.cif
_cod_data_source_block           khriz046
_cod_depositor_comments
'Adding full bibliography for 7716473--7716476.cif.'
_cod_database_code               7716476
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              44624
_shelx_hkl_checksum              55993