Rare antimony(III) imidazole selone complexes: steric controlled structural and bonding aspects.
Nandeshwar, Muneshwar; Adinarayana, Mannem; Srinivas, Katam; Velappan, Kavitha; Prabusankar, Ganesan; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17331–17340; doi:10.1039/d0dt02999h

data_7706090
_publ_section_title
;
 Rare antimony(III) imidazole selone complexes: steric controlled
 structural and bonding aspects.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17331
_journal_page_last               17340
_journal_paper_doi               10.1039/d0dt02999h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C45 H40 Br3 N2 Sb Se, 1[C7H8]'
_chemical_formula_sum            'C52 H48 Br3 N2 Sb Se'
_chemical_formula_weight         1141.404
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2020-09-28
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.09.11 svn.rc89507dd for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2020-10-16 deposited with the CCDC.	2020-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.425(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.17157(19)
_cell_length_b                   23.6916(6)
_cell_length_c                   20.4392(5)
_cell_measurement_reflns_used    7604
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.6970
_cell_measurement_theta_min      3.7280
_cell_volume                     4910.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3-dev (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9798
_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     -2.00  29.00   1.00    1.00    --    0.00 -77.00 -30.00   31
  2  \w    -69.00 -24.00   1.00    1.00    --    0.00 -77.00 -30.00   45
  3  \w    -28.00   8.00   1.00    1.00    --    0.00 -57.00-180.00   36
  4  \w     61.00 108.00   1.00    3.77    --   54.00  57.00-120.00   47
  5  \w     54.00  89.00   1.00    3.77    --   54.00 -99.00-150.00   35
  6  \w     29.00 120.00   1.00    3.77    --   54.00  38.00 -30.00   91
  7  \w     30.00  72.00   1.00    3.77    --   54.00-125.00  60.00   42
  8  \w    -14.00  73.00   1.00    3.77    --   54.00 -57.00  60.00   87
  9  \w      1.00  27.00   1.00    3.77    --   54.00 -99.00-150.00   26
 10  \w     91.00 118.00   1.00    3.77    --  108.00  50.00 -30.00   27
 11  \w     87.00 172.00   1.00    3.77    --  108.00  77.00  30.00   85
 12  \w     37.00 140.00   1.00    3.77    --  108.00 -77.00 -90.00  103
 13  \w     62.00  90.00   1.00    3.77    --  108.00 -50.00 -90.00   28
 14  \w     37.00  85.00   1.00    3.77    --  108.00-111.00-120.00   48
 15  \w    101.00 175.00   1.00    3.77    --  108.00 111.00 -90.00   74
 16  \w    141.00 173.00   1.00    3.77    --  108.00  50.00 -30.00   32
 17  \w     79.00 169.00   1.00    3.77    --  108.00  77.00   0.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.9978
_diffrn_reflns_Laue_measured_fraction_max 0.9798
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18443
_diffrn_reflns_point_group_measured_fraction_full 0.9978
_diffrn_reflns_point_group_measured_fraction_max 0.9798
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         70.13
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    8.427
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2250.228
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.8472
_refine_diff_density_min         -1.0037
_refine_diff_density_rms         0.0827
_refine_ls_d_res_high            0.8197
_refine_ls_d_res_low             15.4494
_refine_ls_goodness_of_fit_ref   1.0298
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     473
_refine_ls_number_reflns         9149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0298
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+1.2632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                7397
_reflns_number_total             9149
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt02999h2.cif
_cod_data_source_block           4
_cod_original_cell_volume        4910.78(19)
_cod_original_formula_sum        'Br3 C52 H48 N2 Sb1 Se1 '
_cod_database_code               7706090
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C33(H33)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C27(H27), C29(H29),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45)
2.c Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C31(H31a,H31b,H31c), C32(H32a,H32b,
 H32c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 224 electrons were 
found in a volume of 1076\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1[C7H8] per Formula Unit 
which account for 200 electrons per unit cell.
;
_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
;