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_7129630
_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 C16 F36 O4'
_chemical_formula_sum            'C36 H30 Al F36 O4 Sb'
_chemical_formula_weight         1359.33
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2022-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.9078(2)
_cell_length_b                   20.33870(10)
_cell_length_c                   22.0435(2)
_cell_measurement_reflns_used    57894
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      75.0050
_cell_measurement_theta_min      2.9730
_cell_volume                     9665.55(14)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(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 0.999
_diffrn_measured_fraction_theta_max 0.986
_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     25.00  70.00   0.50    0.20    --   62.52 -95.00 -30.00   90
  2  \w     31.00  57.00   0.50    0.20    --   62.52  15.00  60.00   52
  3  \w     25.00  71.00   0.50    0.20    --   62.52 -95.00 120.00   92
  4  \w     34.00  63.00   0.50    0.20    --   62.52 -95.00 -60.00   58
  5  \w     61.00 108.00   0.50    0.20    --   62.52  15.00  60.00   94
  6  \w     40.00  67.00   0.50    0.20    --   62.52 -95.00-150.00   54
  7  \w    -54.00 -27.00   0.50    0.20    --  -70.22 125.00 150.00   54
  8  \w    -99.00 -64.00   0.50    0.20    --  -70.22 125.00 150.00   70
  9  \w   -115.00 -57.00   0.50    0.20    --  -70.22 -15.00  30.00  116
 10  \w     48.00  74.00   0.50    0.20    --   75.28 -95.00 -60.00   52
 11  \w   -110.00 -83.00   0.50    0.20    --  -75.50 -71.00 -11.98   54
 12  \w     58.00  84.00   0.50    0.20    --   75.56 -95.00 -90.00   52
 13  \w     51.00  77.00   0.50    0.20    --   75.56 -95.00  30.00   52
 14  \w     71.00  96.00   0.50    0.20    --   75.56-125.00 -30.00   50
 15  \w     76.00 102.00   0.50    0.20    --   78.00-115.00-165.85   52
 16  \w     88.00 116.00   0.50    0.20    --   79.50  34.00 -48.96   56
 17  \w     91.00 122.00   0.50    0.20    --   79.50  19.00 -22.10   62
 18  \w     40.00  82.00   0.50    0.20    --   79.50-102.00 179.34   84
 19  \w     50.00 100.00   0.50    0.20    --   79.50  18.00  89.75  100
 20  \w     48.00 100.00   0.50    0.20    --   79.50  15.00 -48.15  104
 21  \w     44.00  99.00   0.50    0.20    --   79.50-110.00-138.46  110
 22  \w     58.00 106.00   0.50    0.20    --   79.50-127.00  55.15   96
 23  \w     82.00 119.00   0.50    0.20    --   79.50  22.00  16.70   74
 24  \w     43.00  76.00   0.50    0.20    --   79.50-113.00-102.52   66
 25  \w     73.00 122.00   0.50    0.20    --   79.50  22.00 174.37   98
 26  \w     52.00 101.00   0.50    0.20    --   79.50   3.00-112.09   98
 27  \w     58.00  85.00   0.50    0.20    --   79.50 170.00  43.65   54
 28  \w     95.00 122.00   0.50    0.20    --   79.50  12.00 153.06   54
 29  \w     75.00 122.00   0.50    0.20    --   79.50  22.00-127.27   94
 30  \w     50.00  77.00   0.50    0.20    --   79.50  -2.00  -1.75   54
 31  \w     44.00  79.00   0.50    0.20    --   79.50 -90.00 -16.45   70
 32  \w     50.00 100.00   0.50    0.20    --   79.50-122.00 -10.50  100
 33  \w     70.00 118.00   0.50    0.20    --   79.50-145.00 -52.53   96
;
_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      -0.0312771000
_diffrn_orient_matrix_UB_12      -0.0314078000
_diffrn_orient_matrix_UB_13      -0.0612471000
_diffrn_orient_matrix_UB_21      -0.0419500000
_diffrn_orient_matrix_UB_22      0.0607409000
_diffrn_orient_matrix_UB_23      -0.0141003000
_diffrn_orient_matrix_UB_31      0.0486425000
_diffrn_orient_matrix_UB_32      0.0322623000
_diffrn_orient_matrix_UB_33      -0.0330831000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24123
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.523
_diffrn_reflns_theta_min         2.049
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.383
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_description       block
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.121
_refine_diff_density_min         -1.294
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2092
_refine_ls_number_reflns         24123
_refine_ls_number_restraints     1980
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+23.8734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22178
_reflns_number_total             24123
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9886\% 
around [0.70 -0.00 0.71] (reciprocal) or [0.71 -0.00 0.71] (direct)
;
_cod_data_source_file            d1cc06770b2.cif
_cod_data_source_block           heve252_tw_2_abs_twin1_hklf4
_cod_database_code               7129630
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H30 Sb Al O4 F36'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8
 0.2
2. Restrained distances
 C58C-C57
 1.55 with sigma of 0.02
 C59C-C57
 1.55 with sigma of 0.02
 C58B-C57
 1.55 with sigma of 0.02
 F37A-C58A \\sim F37B-C58B \\sim F38B-C58B \\sim F38A-C58A \\sim F39C-C58C
\\sim F37C-C58C \\sim F38C-
 C58C \\sim F39B-C58B \\sim F39A-C58A
 with sigma of 0.02
 F39C-F37C \\sim F37C-F38C \\sim F38C-F39C
 with sigma of 0.02
 F71B-C72B \\sim F70B-C72B \\sim F70C-C72C \\sim F72C-C72C \\sim F70A-C72A
\\sim F71C-C72C \\sim F72B-
 C72B \\sim F71A-C72A \\sim F72A-C72A
 with sigma of 0.02
 F65B-C70B \\sim F66A-C70A \\sim F66B-C70B \\sim F59B-C66B \\sim F65A-C70A
\\sim F65C-C70C \\sim F64A-
 C70A \\sim F64B-C70B \\sim F64C-C70C \\sim F66C-C70C
 with sigma of 0.02
 F67A-C71A \\sim F68A-C71A \\sim F67B-C71B \\sim F68B-C71B \\sim F69B-C71B
\\sim F68C-C71C \\sim F67C-
 C71C \\sim F69A-C71A \\sim F69C-C71C
 with sigma of 0.02
 C71C-C69 \\sim C71A-C69 \\sim C71B-C69 \\sim C70C-C69 \\sim C70A-C69 \\sim
C70B-C69 \\sim C72C-C69 ~
 C72A-C69 \\sim C72B-C69
 with sigma of 0.04
 F40C-C59C \\sim F42C-C59C \\sim F41C-C59C \\sim F41B-C59B \\sim F40B-C59B
\\sim F41A-C59A \\sim F40A-
 C59A \\sim F42A-C59A \\sim F42B-C59B
 with sigma of 0.02
 F44C-C60C \\sim F43C-C60C \\sim F45C-C60C \\sim F44B-C60B \\sim F44A-C60A
\\sim F43B-C60B \\sim F43A-
 C60A \\sim F45B-C60B \\sim F45A-C60A
 with sigma of 0.02
 C65-C67A \\sim C67B-C65 \\sim C65-C66A \\sim C66B-C65 \\sim C68A-C65 \\sim
C68B-C65
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F38C \\sim C58C \\sim F37B \\sim F37A \\sim F37C \\sim F38A \\sim F38B \\sim
F39C \\sim C58B \\sim C58A \\sim F39B \\sim F39A: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.7A
C60A \\sim C60C \\sim C60B \\sim C57 \\sim C59B \\sim C59C \\sim C59A \\sim
C58C \\sim C58B \\sim C58A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F71A \\sim F71B \\sim C72B \\sim F72B \\sim F71C \\sim C72A \\sim C72C \\sim
F70B \\sim F70C \\sim F70A \\sim F72C: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F44C \\sim C60C \\sim F45C \\sim F44A \\sim C60A \\sim F43B \\sim F43C \\sim
F43A \\sim C60B \\sim F45A \\sim F45B \\sim F44B: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.7A
F41C \\sim C59C \\sim F41B \\sim F40C \\sim F40A \\sim C59B \\sim F40B \\sim
F42B \\sim C59A \\sim F42C \\sim F42A \\sim F41A: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.7A
C69 \\sim C70B \\sim C70A \\sim C70C \\sim C71B \\sim C71A \\sim C71C \\sim
C72B \\sim C72C \\sim C72A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C70B \\sim F64B \\sim F65B \\sim F66A \\sim C70A \\sim F65A \\sim F66B \\sim
F64A \\sim F65C \\sim C70C \\sim F66C \\sim F64C: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 1.7A
F68A \\sim F68B \\sim C71B \\sim C71A \\sim F69A \\sim F67C \\sim F67B \\sim
F67A \\sim F68C \\sim F69B \\sim C71C \\sim F69C: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 1.7A
F60B \\sim C66B \\sim F58B \\sim F59B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C65 \\sim O7B \\sim O7A \\sim C67A \\sim C67B \\sim C66A \\sim C66B \\sim C68B
\\sim C68A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
F57B \\sim C68B \\sim F56B \\sim F55B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C51B \\sim C51A \\sim C49 \\sim C52B \\sim C52A \\sim C50B \\sim C50A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F62B \\sim F63B \\sim C67B \\sim F61B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F19A \\sim F19B \\sim C50B \\sim C50A \\sim F21B \\sim F20A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F26A \\sim F27B \\sim C52B \\sim C52A \\sim F25A \\sim F25B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
O8B \\sim O8C \\sim O8A \\sim Al2: within 1.9A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 1.9A
F23A \\sim F24B \\sim C51A \\sim C51B \\sim F22B \\sim F22A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F27A \\sim F20B \\sim C50B \\sim C52A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C51A \\sim F24A \\sim F26B \\sim C52B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
4. Others
 Fixed Sof: F20A(0.64) F22A(0.64) F26A(0.64) F23A(0.64) F19A(0.64) F25A(0.64)
 F27A(0.64) F21A(0.64) F24A(0.64) C52A(0.64) C50A(0.64) C51A(0.64) C58A(0.45)
 F39A(0.45) F37A(0.45) F38A(0.45) C60A(0.45) F44A(0.45) F45A(0.45) F43A(0.45)
 C59A(0.45) F42A(0.45) F40A(0.45) F41A(0.45) O8A(0.48) C70A(0.48) F65A(0.48)
 F64A(0.48) F66A(0.48) C72A(0.48) F71A(0.48) F72A(0.48) F70A(0.48) C71A(0.48)
 F69A(0.48) F67A(0.48) F68A(0.48) O7A(0.6) C68A(0.6) F63A(0.6) F62A(0.6)
 C67A(0.6) F59A(0.6) F60A(0.6) F58A(0.6) C66A(0.6) F57A(0.6) F55A(0.6)
 F56A(0.6) O8B(0.19) C70B(0.21) F66B(0.21) F64B(0.21) F65B(0.21) C72B(0.21)
 F71B(0.21) F72B(0.21) F70B(0.21) C71B(0.21) F69B(0.21) F67B(0.21) F68B(0.21)
 O8C(0.33) C70C(0.31) F66C(0.31) F64C(0.31) F65C(0.31) C72C(0.31) F71C(0.31)
 F72C(0.31) F70C(0.31) C71C(0.31) F69C(0.31) F67C(0.31) F68C(0.31) C58C(0.21)
 F39C(0.21) F37C(0.21) F38C(0.21) C60C(0.21) F44C(0.21) F45C(0.21) F43C(0.21)
 C59C(0.21) F42C(0.21) F40C(0.21) F41C(0.21) C58B(0.34) F39B(0.34) F37B(0.34)
 F38B(0.34) C60B(0.34) F44B(0.34) F45B(0.34) F43B(0.34) C59B(0.34) F42B(0.34)
 F40B(0.34) F41B(0.34) O7B(0.4) C68B(0.4) F57B(0.4) F56B(0.4) C67B(0.4)
 F62B(0.4) F63B(0.4) F61B(0.4) C66B(0.4) F60B(0.4) F58B(0.4) F59B(0.4)
 C50B(0.36) F21B(0.36) F19B(0.36) F20B(0.36) C52B(0.36) F26B(0.36) F27B(0.36)
 F25B(0.36) C51B(0.36) F24B(0.36) F22B(0.36) F23B(0.36)
5.a Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C38(H38A,H38B,H38C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C40(H40A,
 H40B,H40C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C),
 C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C29(H29A,H29B,H29C), C37(H37A,H37B,
 H37C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              73836
_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 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.500
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2