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_4087314
_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, C15 H37 Cr N3 P'
_chemical_formula_sum            'C15 H34 Cr F6 N3 P Sb'
_chemical_formula_weight         575.17
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9265(3)
_cell_length_b                   13.8933(3)
_cell_length_c                   26.2428(7)
_cell_measurement_reflns_used    1288
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.01
_cell_measurement_theta_min      3.37
_cell_volume                     5070.6(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35515
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.353
_diffrn_reflns_theta_min         3.178
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.025
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1069 before and 0.0817 after correction.
 The Ratio of minimum to maximum transmission is 0.61.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 13221 reflections, Rint = 0.1131
 (2527 with I > 3sig(I), Rint = 0.0662)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.109
_refine_diff_density_max         2.487
_refine_diff_density_min         -2.714
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0974
_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^)+(0.0673P)^2^+149.3690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2543
_refine_ls_wR_factor_ref         0.2647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6918
_reflns_number_total             8982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00839_si_002.cif
_cod_data_source_block           best
_cod_database_code               4087314
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.331
_shelx_estimated_absorpt_t_min   0.174
_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. Uiso/Uaniso restraints and constraints
Uanis(C4B) = Uanis(C4A) = Uanis(C10B) = Uanis(C7A)
Uanis(C4B) = Uanis(C4A)
Uanis(C10B) = Uanis(C10A)
3.a Ternary CH refined with riding coordinates:
 C1A(H1A), C4A(H4A), C7A(H7A), C10A(H10A), C1B(H1B), C4B(H4B), C7B(H7B),
 C10B(H10B)
3.b Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C2AA(H2AD,
 H2AE,H2AF), C3A(H3AA,H3AB,H3AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC),
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C11A(H11A,H11B,H11C), C12A(H12A,H12B,
 H12C), C2B(H2BA,H2BB,H2BC), C3B(H3BA,H3BB,H3BC), C5B(H5BA,H5BB,H5BC), C6B(H6BA,
 H6BB,H6BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C11B(H11D,H11E,H11F),
 C12B(H12D,H12E,H12F), C13B(H13A,H13B,H13C), C14B(H14A,H14B,H14C), C15B(H15A,
 H15B,H15C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'