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_7706088
_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         '2(Cl3 Sb), C69 H54 N2 Se, 1[C7H8]'
_chemical_formula_sum            'C76 H62 Cl6 N2 Sb2 Se'
_chemical_formula_weight         1538.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_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                 93.718(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6000(3)
_cell_length_b                   23.7029(6)
_cell_length_c                   22.3885(6)
_cell_measurement_reflns_used    8323
_cell_measurement_temperature    298
_cell_measurement_theta_max      69.9560
_cell_measurement_theta_min      5.3510
_cell_volume                     7202.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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     32.00 123.00   1.00    7.69    --   54.00  57.00  90.00   91
  2  \w    100.00 135.00   1.00    7.69    --  108.00 111.00 120.00   35
  3  \w    115.00 169.00   1.00    7.69    --  108.00 111.00  90.00   54
  4  \w    109.00 164.00   1.00    7.69    --  108.00 111.00  60.00   55
  5  \w    122.00 148.00   1.00    7.69    --  108.00 111.00 -60.00   26
  6  \w    126.00 177.00   1.00    7.69    --  108.00 111.00 -90.00   51
  7  \w    101.00 174.00   1.00    7.69    --  108.00 111.00 -30.00   73
  8  \w     83.00 176.00   1.00    7.69    --  108.00  64.00   0.00   93
  9  \w     82.00 175.00   1.00    7.69    --  108.00  77.00  30.00   93
 10  \w     68.00  93.00   1.00    7.69    --   54.00  57.00 -90.00   25
 11  \w     33.00 109.00   1.00    7.69    --   54.00  57.00-180.00   76
 12  \w     26.00  73.00   1.00    1.92    --    0.00  38.00-120.00   47
 13  \w     98.00 143.00   1.00    7.69    --  108.00 -92.00 -90.00   45
 14  \w     56.00  81.00   1.00    7.69    --   54.00-125.00-150.00   25
 15  \w    -15.00  75.00   1.00    7.69    --   54.00 -57.00 -60.00   90
 16  \w    -27.00  20.00   1.00    1.92    --    0.00  38.00-120.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8286
_diffrn_reflns_point_group_measured_fraction_full 0.618
_diffrn_reflns_point_group_measured_fraction_max 0.606
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.987
_diffrn_reflns_theta_min         3.730
_exptl_absorpt_coefficient_mu    8.895
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.023(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         8286
_refine_ls_number_restraints     626
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0735
_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^)+(0.1648P)^2^+7.2202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2231
_refine_ls_wR_factor_ref         0.2278
_reflns_Friedel_coverage         0.232
_reflns_Friedel_fraction_full    0.237
_reflns_Friedel_fraction_max     0.228
_reflns_number_gt                7687
_reflns_number_total             8286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02999h2.cif
_cod_data_source_block           1
_cod_database_code               7706088
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.176
_shelx_estimated_absorpt_t_min   0.125
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.882(7)
 0.118(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C60) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Ternary CH refined with riding coordinates:
 C11(H11), C24(H24), C44(H44), C57(H57)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C2(H2), C6(H6), C39(H39), C27(H27), C50(H50), C30(H30),
 C46(H46), C68(H68), C59(H59), C36(H36), C41(H41), C34(H34), C26(H26), C49(H49),
  C62(H62), C47(H47), C17(H17), C29(H29), C52(H52), C15(H15), C32(H32),
 C63(H63), C28(H28), C55(H55), C54(H54), C56(H56), C65(H65), C13(H13), C14(H14),
  C33(H33), C48(H48), C69(H69), C19(H19), C53(H53), C35(H35), C20(H20),
 C60(H60), C66(H66), C61(H61), C21(H21), C16(H16), C67(H67)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C43(H43A,H43B,H43C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48652
_shelx_fab_checksum              55475
_platon_squeeze_special_details
;
A solvent mask was calculated and 236 electrons were 
found in a volume of 1224\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 1[C7H8] per Formula Unit 
which account for 200 electrons per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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
;