Synthesis of polyantimony ligand complexes starting from Cp*4Sb4
Heinl, Veronika; Balázs, Gábor; Seidl, Michael; Scheer, Manfred; Chemical Communications  (2022) –; doi:10.1039/D1CC06770B

data_7129634
_publ_section_title
;
 Synthesis of polyantimony ligand complexes starting from Cp*4Sb4
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06770B
_journal_year                    2022
_chemical_formula_moiety         'C20 H30 Sb, Al C36 F46 O3, 1[CH2Cl2]'
_chemical_formula_sum            'C57 H32 Al Cl2 F46 O3 Sb'
_chemical_formula_weight         1858.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2022-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.162(2)
_cell_angle_beta                 100.136(2)
_cell_angle_gamma                105.0430(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0472(2)
_cell_length_b                   14.3850(2)
_cell_length_c                   17.8721(4)
_cell_measurement_reflns_used    34908
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8240
_cell_measurement_theta_min      2.4720
_cell_volume                     3184.65(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.940
_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     24.00  83.00   0.50    0.10    --   62.52-135.00 -52.00  118
  2  \w     36.00  61.00   0.50    0.10    --   62.52-135.00 127.00   50
  3  \w    -74.00 -22.00   0.50    0.10    --  -63.96 135.00  13.00  104
  4  \w    -75.00 -21.00   0.50    0.10    --  -63.96 135.00-166.00  108
  5  \w   -104.00 -39.00   0.50    0.10    --  -70.22 135.00-166.00  130
  6  \w   -103.00 -38.00   0.50    0.10    --  -70.22 135.00  13.00  130
  7  \w     72.00 107.00   0.50    0.10    --   73.14-135.00 -52.00   70
  8  \w     64.00 106.00   0.50    0.10    --   73.14-135.00 127.00   84
  9  \w     82.00 108.00   0.50    0.10    --   75.28-135.00 127.00   52
 10  \w     72.00 107.00   0.50    0.10    --   75.28 135.00  13.00   70
 11  \w     72.00  98.00   0.50    0.10    --   75.28 135.00-166.00   52
 12  \w     83.00 109.00   0.50    0.10    --   75.28-135.00 -52.00   52
 13  \w     37.00  69.00   0.50    0.10    --   34.00  77.00   6.87   64
 14  \w     37.00  62.00   0.50    0.10    --   34.00  77.00-177.85   50
 15  \w    -74.00 -47.00   0.50    0.10    --  -38.00 -74.00-179.62   54
 16  \w     48.00  77.00   0.50    0.10    --   46.00  79.00 120.57   58
 17  \w     66.00  92.00   0.50    0.10    --   58.00  69.00 -67.43   52
 18  \w   -104.00 -74.00   0.50    0.10    --  -62.00 -58.00  24.45   60
 19  \w   -107.00 -76.00   0.50    0.10    --  -66.00 -57.00 162.44   62
 20  \w   -109.00 -80.00   0.50    0.10    --  -66.00 -39.00-149.65   58
 21  \w   -108.00 -78.00   0.50    0.10    --  -66.00 -58.00  83.59   60
 22  \w   -108.00 -76.00   0.50    0.10    --  -66.00 -54.00 -12.06   64
 23  \w   -106.00 -76.00   0.50    0.10    --  -70.00 -74.00 151.80   60
 24  \w   -115.00 -84.00   0.50    0.10    --  -70.00 -39.00-174.71   62
 25  \w   -114.00 -83.00   0.50    0.10    --  -70.00 -40.00  91.63   62
 26  \w   -113.00 -80.00   0.50    0.10    --  -70.00 -54.00 -49.25   66
 27  \w     30.00 102.00   0.50    0.10    --   73.14-125.00   0.00  144
 28  \w     36.00 111.00   0.50    0.10    --   73.14   0.00 150.00  150
 29  \w     38.00 112.00   0.50    0.10    --   75.28   0.00 -90.00  148
 30  \w     33.00 104.00   0.50    0.10    --   75.28-125.00-120.00  142
 31  \w     32.00 104.00   0.50    0.10    --   75.28-125.00 -30.00  144
 32  \w   -110.00 -77.00   0.50    0.10    --  -75.50 -79.00  51.76   66
 33  \w     88.00 125.00   0.50    0.10    --   77.54  36.00 -20.05   74
 34  \w     34.00 103.00   0.50    0.10    --   77.54-118.00  34.26  138
 35  \w     67.00 123.00   0.50    0.10    --   77.54  23.00 172.93  112
 36  \w     34.00 107.00   0.50    0.10    --   77.54-127.00 174.21  146
 37  \w     98.00 124.00   0.50    0.10    --   77.54  36.00 -57.12   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0107744000
_diffrn_orient_matrix_UB_12      0.0232157000
_diffrn_orient_matrix_UB_13      -0.0828105000
_diffrn_orient_matrix_UB_21      0.0999686000
_diffrn_orient_matrix_UB_22      0.0841942000
_diffrn_orient_matrix_UB_23      0.0288142000
_diffrn_orient_matrix_UB_31      0.0731913000
_diffrn_orient_matrix_UB_32      -0.0685730000
_diffrn_orient_matrix_UB_33      0.0000972000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41998
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.264
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.039
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_description       plate
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         12196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+2.9392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11866
_reflns_number_total             12196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06770b2.cif
_cod_data_source_block           heve351_ap_abs_gaus
_cod_database_code               7129634
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AlC57Cl2F46H32O3Sb
_shelx_estimated_absorpt_t_max   0.713
_shelx_estimated_absorpt_t_min   0.273
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C8(H8A,H8B,
 H8C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C9(H9A,H9B,H9C), C7(H7A,H7B,
 H7C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 84 electrons were 
found in a volume of 220\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH2Cl2] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78498
_shelx_fab_checksum              59724
_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 1.999
_oxdiff_exptl_absorpt_empirical_full_min 0.629