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_7706091
_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 Cl3 N2 Sb Se, 1[C7H8]'
_chemical_formula_sum            'C52 H48 Cl3 N2 Sb Se'
_chemical_formula_weight         1008.051
_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                 104.844(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0909(3)
_cell_length_b                   20.4357(4)
_cell_length_c                   17.3498(4)
_cell_measurement_reflns_used    8226
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      69.6850
_cell_measurement_theta_min      3.2280
_cell_volume                     4829.27(18)
_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 0.9952
_diffrn_measured_fraction_theta_max 0.9777
_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    -35.00  17.00   1.00    1.00    --    0.00 -57.00 -60.00   52
  2  \w    -69.00 -44.00   1.00    1.00    --    0.00 -57.00 -60.00   25
  3  \w     36.00  61.00   1.00    1.00    --    0.00  57.00 -30.00   25
  4  \w    -22.00  25.00   1.00    1.00    --    0.00  57.00-180.00   47
  5  \w     25.00  99.00   1.00    3.13    --   54.00-125.00   0.00   74
  6  \w     76.00 103.00   1.00    3.13    --   54.00  57.00  60.00   27
  7  \w     31.00 125.00   1.00    3.13    --   54.00  77.00 -90.00   94
  8  \w    -16.00  85.00   1.00    3.13    --   54.00 -77.00  30.00  101
  9  \w     82.00 108.00   1.00    3.13    --   54.00  57.00-180.00   26
 10  \w    104.00 156.00   1.00    3.13    --  108.00 107.00-121.00   52
 11  \w     47.00  75.00   1.00    3.13    --  108.00-111.00-150.00   28
 12  \w     88.00 166.00   1.00    3.13    --  108.00  63.00 120.00   78
 13  \w    108.00 135.00   1.00    3.13    --  108.00 -38.00 150.00   27
 14  \w     43.00  92.00   1.00    3.13    --  108.00 -38.00 -60.00   49
 15  \w     79.00 151.00   1.00    3.13    --  108.00 178.00 -60.00   72
 16  \w     61.00 147.00   1.00    3.13    --  108.00 178.00  30.00   86
 17  \w    126.00 171.00   1.00    3.13    --  108.00 111.00  90.00   45
 18  \w     41.00 114.00   1.00    3.13    --  108.00 -77.00  30.00   73
;
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.9952
_diffrn_reflns_Laue_measured_fraction_max 0.9777
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18971
_diffrn_reflns_point_group_measured_fraction_full 0.9952
_diffrn_reflns_point_group_measured_fraction_max 0.9777
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         69.96
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    7.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69843
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2046.685
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.3510
_refine_diff_density_min         -0.4602
_refine_diff_density_rms         0.0679
_refine_ls_d_res_high            0.8206
_refine_ls_d_res_low             13.6206
_refine_ls_goodness_of_fit_ref   1.0202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    95
_refine_ls_number_parameters     582
_refine_ls_number_reflns         8956
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      0.9945
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.2640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                7344
_reflns_number_total             8956
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt02999h2.cif
_cod_data_source_block           3
_cod_original_cell_volume        4829.23(17)
_cod_original_formula_sum        'C52 Cl3 H48 N2 Sb1 Se1 '
_cod_database_code               7706091
_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
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C12-C13 \\sim C12-C13A
 with sigma of 0.02
 C12-C19 \\sim C12-C19A
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C13-C18 \\sim C13A-C18A
 with sigma of 0.02
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C18-C17 \\sim C18A-C17A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C16-C17 \\sim C16A-C17A
 with sigma of 0.02
 C15-C17 \\sim C15A-C17A
 with sigma of 0.04
 C19-C24 \\sim C19A-C24A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C19-C23 \\sim C19A-C23A
 with sigma of 0.04
 C24-C23 \\sim C24A-C23A
 with sigma of 0.02
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C23-C22 \\sim C23A-C22A
 with sigma of 0.02
 C24-C20 \\sim C24A-C20A
 with sigma of 0.04
 C24-C22 \\sim C24A-C22A
 with sigma of 0.04
 C12-C14 \\sim C12-C14A
 with sigma of 0.04
 C12-C18 \\sim C12-C18A
 with sigma of 0.04
 C12-C24 \\sim C12-C24A
 with sigma of 0.04
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
 C12-C20 \\sim C12-C20A
 with sigma of 0.04
 C13-C15 \\sim C13A-C15A
 with sigma of 0.04
 C13-C17 \\sim C13A-C17A
 with sigma of 0.04
 C14-C18 \\sim C14A-C18A
 with sigma of 0.04
 C14-C16 \\sim C14A-C16A
 with sigma of 0.04
 C18-C16 \\sim C18A-C16A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C4, C12, C13, C9, C8, C7, C5, C14, C6, C18, C15, C16, C17, C19, C24, C20, C21,
  C23, C22, C11, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 H12, H20, C19, C13, H23, C14, H24, H14, H21, C18, H22, H18, C24, C15, C20,
 H15, C21, C16, C23, H16, C22, C17, H17, C9, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 H12a, H20A, C19A, C13A, H23A, C14A, H24A, H14A, H21A, C18A, H22A, H18A, C24A,
 C15A, C20A, H15A, C21A, C16A, C23A, H16A, C22A, C17A, H17A, C9, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H12a)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C18A)=Sof(H18A)=Sof(C15A)=
 Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C19A)=Sof(C24A)=
 Sof(H24A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C23A)=Sof(H23A)=
 Sof(C22A)=Sof(H22A)=1-FVAR(1)
 Sof(H12)=Sof(C13)=Sof(C14)=Sof(H14)=Sof(C18)=Sof(H18)=Sof(C15)=Sof(H15)=
 Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C19)=Sof(C24)=Sof(H24)=Sof(C20)=
 Sof(H20)=Sof(C21)=Sof(H21)=Sof(C23)=Sof(H23)=Sof(C22)=Sof(H22)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C12(H12a), C33(H33)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C27(H27), C41(H41), C14(H14), C42(H42), C29(H29), C45(H45),
 C6(H6), C3(H3), C18(H18), C15(H15), C16(H16), C44(H44), C17(H17), C43(H43),
 C39(H39), C35(H35), C38(H38), C24(H24), C36(H36), C37(H37), C20(H20), C21(H21),
  C23(H23), C22(H22), C14A(H14A), C18A(H18A), C15A(H15A), C16A(H16A),
 C17A(H17A), C24A(H24A), C20A(H20A), C21A(H21A), C23A(H23A), C22A(H22A)
6.c Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C32(H32a,H32b,
 H32c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 208 electrons were 
found in a volume of 968\%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
;