Weakly Coordinating yet Ion Paired: Anion Effects on an Internal Rearrangement
Aldrich, Kelly E.; Billow, Brennan S.; Holmes, Daniel; Bemowski, Ross D.; Odom, Aaron L.; Organometallics 36 (2017) 1227–; doi:10.1021/acs.organomet.6b00839

data_4087316
_publ_section_title
;
 Weakly Coordinating yet Ion Paired: Anion Effects on an Internal
 Rearrangement
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1227
_journal_paper_doi               10.1021/acs.organomet.6b00839
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'F6 Sb, C20 H39 Cr N3 P'
_chemical_formula_sum            'C20 H39 Cr F6 N3 P Sb'
_chemical_formula_weight         640.26
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_symmetry_space_group_name_Hall  'P -2ac -2n'
_symmetry_space_group_name_H-M   'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.733(2)
_cell_length_b                   10.254(2)
_cell_length_c                   27.719(6)
_cell_measurement_reflns_used    9177
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.599
_cell_measurement_theta_min      2.118
_cell_volume                     2766.4(10)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40057
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.622
_diffrn_reflns_theta_min         2.118
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0838 before and 0.0713 after correction.
The Ratio of minimum to maximum transmission is 0.9203.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       needle
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0176P)^2^+3.3125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0740
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.927
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                3548
_reflns_number_total             4620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00839_si_002.cif
_cod_data_source_block           bsb-ii-32
_cod_depositor_comments
;

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         320.13
_cod_original_formula_moiety         '0.5(F6 Sb), 0.5(C20 H39 Cr N3 P)'
_cod_original_formula_units_Z            8
_cod_original_cell_volume        2766.3(10)
_cod_original_formula_sum        'C10 H19.50 Cr0.50 F3 N1.50 P0.50 Sb0.50'
_cod_database_code               4087316
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.689
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.64(4) 0.36(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C5(H5), C15(H15), C3(H3), C2AA(H2AA)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C1(H1), C2(H2), C1AA(H1AA)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C51(H51A,H51B,H51C), C0AA(H0AA,H0AB,
 H0AC), C11(H11A,H11B,H11C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C3AA(H3AA,H3AB,
 H3AC), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'