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_7703267
_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         'C31 H39 F N2 Sb, B C24 F20, 0.5(C6 H4 F2)'
_chemical_formula_sum            'C58 H41 B F22 N2 Sb'
_chemical_formula_weight         1316.49
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-25
_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
_cell_angle_beta                 113.5290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2924(2)
_cell_length_b                   17.8036(2)
_cell_length_c                   17.4223(2)
_cell_measurement_reflns_used    18180
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      71.6200
_cell_measurement_theta_min      3.8510
_cell_volume                     5202.19(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.987
_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   -101.00 -17.00   1.00    5.00    --  -33.50 -57.00  90.00   84
  2  \w    -31.00  53.00   1.00    5.00    --   36.58 -57.00 120.00   84
  3  \w     18.00  90.00   1.00    5.00    --   36.58-125.00  90.00   72
  4  \w     20.00 104.00   1.00    5.00    --   36.58  57.00 -90.00   84
  5  \w    -31.00  53.00   1.00    5.00    --   36.58 -57.00 150.00   84
  6  \w     70.00 178.00   1.00   20.00    --  108.00  15.00 -60.00  108
  7  \w     38.00 129.00   1.00   20.00    --  108.00 -30.00  90.00   91
  8  \w     90.00 175.00   1.00   20.00    --  108.00  61.00 -90.00   85
  9  \w     41.00 126.00   1.00   20.00    --  108.00 -61.00-120.00   85
 10  \w     39.00 109.00   1.00   20.00    --  108.00 -94.00   0.00   70
 11  \w     40.00 125.00   1.00   20.00    --  108.00 -45.00 -30.00   85
 12  \w     37.00 146.00   1.00   20.00    --  108.00 -15.00 -90.00  109
 13  \w     41.00 126.00   1.00   20.00    --  108.00 -61.00   0.00   85
 14  \w     17.00 106.00   1.00    5.00    --   36.58  37.00-150.00   89
 15  \w    -31.00  53.00   1.00    5.00    --   36.58 -57.00-120.00   84
 16  \w    -31.00  53.00   1.00    5.00    --   36.58 -57.00 -30.00   84
 17  \w     10.00 104.00   1.00    5.00    --   36.58  77.00   0.00   94
 18  \w     39.00 109.00   1.00   20.00    --  108.00 -94.00-180.00   70
 19  \w     87.00 124.00   1.00   20.00    --  108.00  30.00  30.00   37
 20  \w     87.00 178.00   1.00   20.00    --  108.00  30.00  90.00   91
;
_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      -0.0753475000
_diffrn_orient_matrix_UB_12      0.0186664000
_diffrn_orient_matrix_UB_13      -0.0785107000
_diffrn_orient_matrix_UB_21      -0.0463164000
_diffrn_orient_matrix_UB_22      0.0145419000
_diffrn_orient_matrix_UB_23      0.0555164000
_diffrn_orient_matrix_UB_31      0.0249543000
_diffrn_orient_matrix_UB_32      0.0831644000
_diffrn_orient_matrix_UB_33      0.0078377000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38975
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.991
_diffrn_reflns_theta_min         3.621
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.312
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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    1.681
_exptl_crystal_description       block
_exptl_crystal_F_000             2628
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.101
_refine_diff_density_max         1.240
_refine_diff_density_min         -2.636
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         10089
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1362P)^2^+35.0888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2431
_refine_ls_wR_factor_ref         0.2467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9230
_reflns_number_total             10089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00024h3.cif
_cod_data_source_block           Compound5
_cod_depositor_comments
'Adding full bibliography for 7703262--7703267.cif.'
_cod_database_code               7703267
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         Sb1C51H21B1F21N2
_chemical_oxdiff_usercomment     'Light yellow block'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33-F2 \\sim C32-F3
 with sigma of 0.02
 C33-C34 \\sim C35-C34 \\sim C33-C32 \\sim C36-C35 \\sim C37-C36 \\sim C32-C37
 with sigma of 0.02
 C33-F3 \\sim C37-F3 \\sim C32-F2 \\sim C34-F2
 with sigma of 0.04
 C36-C34 \\sim C37-C35 \\sim C32-C36 \\sim C33-C37 \\sim C32-C34 \\sim C33-C35
 with sigma of 0.04
3. Restrained planarity
 C33, C32, C37, C36, C35, C34, F2, F3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C33 \\sim C32 \\sim C37 \\sim C36 \\sim C35 \\sim C34 \\sim F2 \\sim F3: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C33, C32, C37, C36, C35, C34, F2, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C33(0.5) C32(0.5) C37(0.5) H37(0.5) C36(0.5) H36(0.5) C35(0.5)
 H35(0.5) C34(0.5) H34(0.5) F2(0.5) F3(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C31(H31), C15(H15), C22(H22), C24(H24), C13(H13), C37(H37),
 C36(H36), C35(H35), C34(H34)
7.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C26(H26A,H26B,
 H26C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C8(H8A,H8B,H8C), C18(H18A,H18B,
 H18C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_olex2_date_sample_data_collection 2019-10-03
_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.607