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_7706089
_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_absolute_configuration unk
_chemical_formula_moiety
'2(Br3 Sb), C69 H57 N2 Se, 1[C7H8], 0.334[CH2Cl2]'
_chemical_formula_sum            'C76.33 H65.67 Br6 Cl0.67 N2 Sb2 Se'
_chemical_formula_weight         1836.669
_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'
_symmetry_Int_Tables_number      9
_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                 91.6768(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.78581(17)
_cell_length_b                   23.6833(5)
_cell_length_c                   22.4844(4)
_cell_measurement_reflns_used    6232
_cell_measurement_temperature    298
_cell_measurement_theta_max      71.4533
_cell_measurement_theta_min      3.7080
_cell_volume                     7337.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      298.0
_diffrn_detector_area_resol_mean 16.1293
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9839
_diffrn_measurement_details
;
  1 omega  -20.00    7.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  120.0000 27

  2 omega  -70.00  -44.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  120.0000 26

  3 omega  -32.00   29.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000 -120.0000 61

  4 omega -113.00  -77.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -90.0000 36

  5 omega  -65.00   18.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   63.0000  -60.0000 83

  6 omega -116.00  -42.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  178.0000  -90.0000 74

  7 omega   41.00   93.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -       55.1393 -125.0000 -122.0000 52

  8 omega   61.00   94.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -25.0000    0.0000 33

  9 omega   45.00   92.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -25.0000  -30.0000 47

 10 omega   89.00  164.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786   25.0000  150.0000 75

 11 omega  101.00  167.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786  125.0000  -44.0000 66

 12 omega   40.00  103.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -50.0000 -150.0000 63

 13 omega   60.00  116.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000  120.0000 56

 14 omega   64.00   90.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000 -120.0000 26

 15 omega   76.00  106.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -111.0000 -180.0000 30

 16 omega   39.00  116.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786 -125.0000   57.0000 77

 17 omega   46.00   86.00   1.0000    2.1600
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000  150.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9839
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13542
_diffrn_reflns_point_group_measured_fraction_full 0.5590
_diffrn_reflns_point_group_measured_fraction_max 0.5483
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         71.60
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    10.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3570.525
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.3374
_refine_diff_density_min         -0.3816
_refine_diff_density_rms         0.0560
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.046(8)
_refine_ls_d_res_high            0.8125
_refine_ls_d_res_low             11.9105
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   0.9521
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    109
_refine_ls_number_parameters     724
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.9521
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.112
_reflns_limit_h_max              7
_reflns_limit_h_min              -16
_reflns_limit_k_max              28
_reflns_limit_k_min              -28
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                6764
_reflns_number_total             7850
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt02999h2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_original_formula_sum        'Br6 C76.33 Cl0.67 H65.67 N2 Sb2 Se1 '
_cod_database_code               7706089
_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.a Ternary CH refined with riding coordinates:
 C11(H11), C24(H24), C44(H44), C57(H57)
2.b Secondary CH2 refined with riding coordinates:
 C66(H66a,H66b)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C39(H39), C41(H41), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C59(H59), C60(H60),
 C61(H61), C62(H62), C63(H63), C65(H65), C67(H67), C68(H68), C69(H69)
2.d Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C43(H43a,H43b,H43c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 280 electrons were 
found in a volume of 1266\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1[C7H8], 0.333[CH2Cl2] per Formula Unit 
which account for 256 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'