The crystal structure of N,N′-(1,2-phenylene)bis (2-((2-oxopropyl)selanyl)benzamide), C26H24N2O4Se2
Feng, Shuxiao; Zhong, Xuan; Qi, Kaiyan; Guo, Yafei; Wang, Junling; Gu, Guangna; Ma, Junying; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 739–741; doi:10.1515/ncrs-2023-0181

data_8107546
_publ_section_title
;
 The crystal structure of N,N&#x2032;-(1,2-phenylene)bis
 (2-((2-oxopropyl)selanyl)benzamide), C26H24N2O4Se2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              739
_journal_page_last               741
_journal_paper_doi               10.1515/ncrs-2023-0181
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C26 H24 N2 O4 Se2'
_chemical_formula_sum            'C26 H24 N2 O4 Se2'
_chemical_formula_weight         586.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 91.983(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.9092(7)
_cell_length_b                   5.8900(2)
_cell_length_c                   36.6209(9)
_cell_measurement_reflns_used    4143
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.5500
_cell_measurement_theta_min      3.8520
_cell_volume                     4938.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -89.00   2.00   1.00    2.00    --  -33.50 127.00 -28.00   91
  2  \w   -108.00 -32.00   1.00    2.00    --  -33.50 178.00-150.00   76
  3  \w   -108.00 -32.00   1.00    2.00    --  -33.50 178.00   0.00   76
  4  \w    -71.00 -30.00   1.00    2.00    --  -33.50  19.00  60.00   41
  5  \w    -98.00 -18.00   1.00    2.00    --  -33.50 -57.00-120.00   80
  6  \w    -62.00 -32.00   1.00    2.00    --  -33.50 178.00 -60.00   30
  7  \w     45.00  92.00   1.00    2.00    --   36.47-127.00-105.00   47
  8  \w    -26.00  -1.00   1.00    2.00    --   36.47 -57.00 120.00   25
  9  \w     73.00 101.00   1.00    2.00    --   36.47 178.00  30.00   28
 10  \w      0.00  68.00   1.00    2.00    --   36.47  19.00 -60.00   68
 11  \w      8.00  53.00   1.00    2.00    --   36.47 -57.00 120.00   45
 12  \w    -30.00  50.00   1.00    2.00    --   36.47 -77.00 120.00   80
 13  \w     41.00 103.00   1.00    2.00    --   36.47  57.00   0.00   62
 14  \w    -33.00  20.00   1.00    2.00    --   36.47 -77.00  90.00   53
 15  \w     50.00  89.00   1.00    3.00    --  108.00 -45.00-180.00   39
 16  \w    142.00 170.00   1.00    3.00    --  108.00 111.00 150.00   28
 17  \w    107.00 132.00   1.00    3.00    --  108.00 111.00 150.00   25
 18  \w    123.00 153.00   1.00    3.00    --  108.00 111.00-150.00   30
 19  \w     86.00 177.00   1.00    3.00    --  108.00  30.00-120.00   91
 20  \w     92.00 175.00   1.00    3.00    --  108.00  30.00 -30.00   83
 21  \w    151.00 177.00   1.00    3.00    --  108.00 111.00-180.00   26
 22  \w    118.00 145.00   1.00    3.00    --  108.00 111.00-180.00   27
 23  \w     89.00 176.00   1.00    3.00    --  108.00  61.00 -90.00   87
 24  \w     79.00 112.00   1.00    3.00    --  108.00-111.00 -90.00   33
 25  \w     54.00 128.00   1.00    3.00    --  108.00 -45.00  90.00   74
 26  \w     71.00 110.00   1.00    3.00    --  108.00 -94.00  90.00   39
 27  \w     48.00 128.00   1.00    3.00    --  108.00 -61.00-150.00   80
 28  \w     71.00 112.00   1.00    3.00    --  108.00-111.00   0.00   41
 29  \w     86.00 111.00   1.00    3.00    --  108.00 178.00-150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0601961000
_diffrn_orient_matrix_UB_12      -0.0344393000
_diffrn_orient_matrix_UB_13      0.0166658000
_diffrn_orient_matrix_UB_21      -0.0291571000
_diffrn_orient_matrix_UB_22      0.0047570000
_diffrn_orient_matrix_UB_23      -0.0385400000
_diffrn_orient_matrix_UB_31      0.0074656000
_diffrn_orient_matrix_UB_32      -0.2591947000
_diffrn_orient_matrix_UB_33      -0.0029182000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            14718
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.063
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         3.861
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.036
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4379
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+4.2586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3327
_reflns_number_total             4379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0181_suppl_001.cif
_cod_data_source_block           fshx3
_cod_database_code               8107546
_shelx_estimated_absorpt_t_max   0.738
_shelx_estimated_absorpt_t_min   0.622
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 N1-H1
 0.87 with sigma of 0.02
 H2-N2
 0.87 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) = Uanis(O4A)
Uanis(C26) = Uanis(C26A)
4. Others
 Sof(O4A)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(O4)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C26A(H26D,H26E,H26F)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.816