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_7703265
_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, C F3 O3 S'
_chemical_formula_sum            'C21 H30 F3 O3 S Sb'
_chemical_formula_weight         541.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1165(3)
_cell_length_b                   15.8699(3)
_cell_length_c                   16.6561(3)
_cell_measurement_reflns_used    9139
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      30.0230
_cell_measurement_theta_min      3.7260
_cell_volume                     4524.42(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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.935
_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    -47.00  37.00   1.00   20.00    --   20.05 -57.00-120.00   84
  2  \f    244.00 358.00   1.00   20.00 -14.89  20.05   0.00    --   114
  3  \w    -37.00 -12.00   1.00   20.00    --  -19.89  57.00  90.00   25
  4  \w      3.00  87.00   1.00   20.00    --   20.05  57.00  60.00   84
  5  \w     -9.00  91.00   1.00   20.00    --   20.05  19.00   0.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0257604000
_diffrn_orient_matrix_UB_12      0.0208937000
_diffrn_orient_matrix_UB_13      0.0267846000
_diffrn_orient_matrix_UB_21      -0.0324330000
_diffrn_orient_matrix_UB_22      0.0156419000
_diffrn_orient_matrix_UB_23      0.0218922000
_diffrn_orient_matrix_UB_31      0.0008388000
_diffrn_orient_matrix_UB_32      -0.0362748000
_diffrn_orient_matrix_UB_33      0.0248674000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45019
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.926
_diffrn_reflns_theta_min         3.413
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.355
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.753
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 2920 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         12853
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                8678
_reflns_number_total             12853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00024h3.cif
_cod_data_source_block           Compound1a
_cod_depositor_comments
'Adding full bibliography for 7703262--7703267.cif.'
_cod_database_code               7703265
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C21Sb1F3S1O3H30
_chemical_oxdiff_usercomment     'Orange/yellow block'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(4)
 0.50(4)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3.a Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C16(H16A,H16B,H16C), C8(H8A,H8B,
 H8C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C20(H20A,H20B,H20C), C39(H39A,
 H39B,H39C), C36(H36A,H36B,H36C), C29(H29A,H29B,H29C), C9(H9A,H9B,H9C), C6(H6A,
 H6B,H6C), C26(H26A,H26B,H26C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C30(H30A,H30B,H30C),
 C40(H40A,H40B,H40C)
;
_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 1.135
_oxdiff_exptl_absorpt_empirical_full_min 0.887