Diverse structure and reactivity of pentamethylcyclopentadienyl antimony(iii) cations.
Coughlin, Omar; Krämer, Tobias; Benjamin, Sophie L.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 1726–1730; doi:10.1039/d0dt00024h

data_7703264
_publ_section_title
;
 Diverse structure and reactivity of pentamethylcyclopentadienyl
 antimony(iii) cations.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1726
_journal_page_last               1730
_journal_paper_doi               10.1039/d0dt00024h
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C10 H15 Cl Sb, B C24 F20'
_chemical_formula_sum            'C34 H15 B Cl F20 Sb'
_chemical_formula_weight         971.47
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-25 deposited with the CCDC.	2020-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.679(5)
_cell_angle_beta                 96.606(5)
_cell_angle_gamma                104.469(5)
_cell_formula_units_Z            2
_cell_length_a                   10.5921(7)
_cell_length_b                   12.6396(8)
_cell_length_c                   12.8627(8)
_cell_measurement_reflns_used    3642
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.2300
_cell_measurement_theta_min      3.4570
_cell_volume                     1654.89(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_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      6.00  91.00   1.00    2.50    --   20.05  19.00  60.00   85
  2  \w     22.00  87.00   1.00    2.50    --   20.05  57.00 150.00   65
  3  \w     -6.00  46.00   1.00    2.50    --   20.05  77.00   0.00   52
  4  \w      7.00  82.00   1.00    2.50    --   20.05  57.00 -60.00   75
  5  \w    -19.00  59.00   1.00    2.50    --   20.05 -99.00-120.00   78
  6  \w    -82.00   5.00   1.00    2.50    --  -19.97 -77.00  60.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0046169000
_diffrn_orient_matrix_UB_12      0.0374399000
_diffrn_orient_matrix_UB_13      -0.0400381000
_diffrn_orient_matrix_UB_21      -0.0380437000
_diffrn_orient_matrix_UB_22      -0.0435865000
_diffrn_orient_matrix_UB_23      -0.0343179000
_diffrn_orient_matrix_UB_31      -0.0581927000
_diffrn_orient_matrix_UB_32      0.0079573000
_diffrn_orient_matrix_UB_33      0.0175037000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.1266
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17501
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         3.332
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.161
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5535
_reflns_number_total             8897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00024h3.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
'Adding full bibliography for 7703262--7703267.cif.'
_cod_database_code               7703264
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C34 H15 B Cl F20 Sb1'
_chemical_oxdiff_usercomment     'Yellow Block'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C6(H6A,H6B,H6C)
;
_olex2_date_sample_data_collection 2019-02-04
_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 1.089
_oxdiff_exptl_absorpt_empirical_full_min 0.887