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_7703262
_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         'C20 H30 Sb, B C24 F20'
_chemical_formula_sum            'C44 H30 B F20 Sb'
_chemical_formula_weight         1071.24
_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
;
2019-11-26 deposited with the CCDC.	2020-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                108.476(3)
_cell_angle_beta                 104.868(3)
_cell_angle_gamma                103.354(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4426(4)
_cell_length_b                   12.7883(4)
_cell_length_c                   15.2203(5)
_cell_measurement_reflns_used    14563
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.5540
_cell_measurement_theta_min      3.5880
_cell_volume                     2087.32(14)
_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 0.909
_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      3.00  87.00   1.00   10.00    --   19.89  57.00  60.00   84
  2  \w     -7.00  87.00   1.00   10.00    --   19.89  77.00 150.00   94
  3  \w    -25.00  59.00   1.00   10.00    --   19.89 -99.00 -90.00   84
  4  \w    -25.00  59.00   1.00   10.00    --   19.89 -99.00  30.00   84
  5  \w     -7.00  87.00   1.00   10.00    --   19.89  77.00  90.00   94
  6  \w    -47.00  37.00   1.00   10.00    --   19.89 -57.00 150.00   84
  7  \w    -25.00  59.00   1.00   10.00    --   19.89 -99.00 -60.00   84
  8  \w      3.00  87.00   1.00   10.00    --   19.89  57.00 -30.00   84
  9  \w     35.00  92.00   1.00   10.00    --   19.89 178.00-150.00   57
 10  \w    -25.00   0.00   1.00   10.00    --   19.89 -99.00 120.00   25
 11  \w      1.00  89.00   1.00   10.00    --   19.89  37.00 -90.00   88
;
_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      0.0138822000
_diffrn_orient_matrix_UB_12      -0.0197665000
_diffrn_orient_matrix_UB_13      -0.0434073000
_diffrn_orient_matrix_UB_21      0.0413563000
_diffrn_orient_matrix_UB_22      -0.0212094000
_diffrn_orient_matrix_UB_23      0.0240520000
_diffrn_orient_matrix_UB_31      -0.0450813000
_diffrn_orient_matrix_UB_32      -0.0550294000
_diffrn_orient_matrix_UB_33      -0.0174649000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43455
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.797
_diffrn_reflns_theta_min         3.276
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.853
_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            reddish
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         11878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.8341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8896
_reflns_number_total             11878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00024h3.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
'Adding full bibliography for 7703262--7703267.cif.'
_cod_original_cell_volume        2087.32(13)
_cod_database_code               7703262
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         SbC44F20H30B1
_chemical_oxdiff_usercomment     'Orange 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:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C7(H7A,H7B,
 H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_olex2_date_sample_data_collection 2019-04-04
_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 6.394
_oxdiff_exptl_absorpt_empirical_full_min 0.887