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_7716473
_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         'C48 H67 N2 Na O3'
_chemical_formula_sum            'C48 H67 N2 Na O3'
_chemical_formula_weight         743.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 95.5627(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2430(11)
_cell_length_b                   11.4393(6)
_cell_length_c                   18.8683(10)
_cell_measurement_reflns_used    91053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.01
_cell_measurement_theta_min      2.27
_cell_volume                     4348.7(4)
_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 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  0.0673
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            360243
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'microfocus Mo X-ray tube'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9361
_exptl_absorpt_correction_T_min  0.8927
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Stalke et al., 2015)

 Equivalent reflections defined by point group 2/m for scaling and error model
 Mean and maximum errors in direction cosine check function =   0.000   0.004
 Restraint esd for equal adjacent scale factors =  0.0050
 Maximum odd and even orders for spherical harmonics =   1   4

 wR2(int) =  0.1349 (selected reflections only, before parameter refinement)
 wR2(int) =  0.0772 (selected reflections only, after parameter refinement)

  392384 total and  14525 unique reflections assuming Friedel's law
 plus  12059 total and  3658 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)

  386142 total and  14523 unique reflections left after |I-<I>|/su test
 plus  11608 total and  3646 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  25.1  0.0669  0.110 - 0.140  1.017 - 1.052  1.027  0.0436  22.9   26797   16806
   2  28.2  0.0778  0.105 - 0.161  1.018 - 1.058  1.046  0.0436  22.9   26206   15469
   3  25.0  0.0691  0.112 - 0.154  1.017 - 1.051  1.035  0.0436  22.9   23599   14070
   4  25.1  0.0719  0.102 - 0.168  1.017 - 1.052  1.049  0.0436  22.9   26754   16403
   5  25.0  0.0727  0.095 - 0.182  1.017 - 1.056  1.038  0.0436  22.9   25263   14835
   6  25.0  0.0723  0.101 - 0.162  1.018 - 1.058  1.021  0.0436  22.9   25261   15236
   7  25.1  0.0719  0.099 - 0.176  1.017 - 1.054  1.028  0.0436  22.9   23280   13896
   8  25.0  0.0758  0.102 - 0.174  1.017 - 1.052  1.040  0.0436  22.9   25632   15201
   9  25.0  0.0723  0.110 - 0.156  1.017 - 1.054  1.038  0.0436  22.9   26843   16274
  10  25.0  0.0735  0.110 - 0.149  1.018 - 1.054  1.037  0.0436  22.9   26107   15431
  11  25.0  0.0666  0.106 - 0.157  1.017 - 1.052  1.035  0.0436  22.9   26761   16698
  12 -25.1  0.0697  0.096 - 0.166  1.017 - 1.055  1.030  0.0436  22.9   24960   14520
  13 -25.1  0.0677  0.113 - 0.156  1.017 - 1.052  1.026  0.0436  22.9   25604   15661
  14  25.0  0.0649  0.090 - 0.175  1.017 - 1.058  1.046  0.0436  22.9   37448   24164
  15  25.0  0.0660  0.097 - 0.160  1.017 - 1.052  1.066  0.0436  22.9   15627    9592
  16f  0.0  0.1358  0.090 - 0.175  1.018 - 1.053  1.049  0.0436  22.9   11608    5945

       4 Overloads replaced by fast scan measurements
  386146 Corrected reflections written to file hkl
 Estimated minimum and maximum transmission:  0.8927  0.9361
 Additional spherical absorption correction applied with mu*r =  0.0100
 3lambda correction factor = 0.00150
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       plank
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         12718
_refine_ls_number_restraints     466
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0677P)^2^+2.3658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10586
_reflns_number_total             12718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01039f2.cif
_cod_data_source_block           khriz045
_cod_depositor_comments
'Adding full bibliography for 7716473--7716476.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7716473
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              2132
_shelx_hkl_checksum              61645