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_4087315
_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         'C15 H37 Cr N3 P, C32 H12 B F24'
_chemical_formula_sum            'C47 H49 B Cr F24 N3 P'
_chemical_formula_weight         1205.67
_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   mixed
_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                 95.2910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1223(10)
_cell_length_b                   18.1046(13)
_cell_length_c                   23.1296(17)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.18
_cell_volume                     5471.6(7)
_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)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.999
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44965
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.386
_diffrn_reflns_theta_min         1.431
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0548 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9082.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       cube
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         10039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0910P)^2^+8.8382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7239
_reflns_number_total             10039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00839_si_002.cif
_cod_data_source_block           final
_cod_database_code               4087315
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.909
_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(F5A) = Uanis(F5B)
Uanis(F6B) = Uanis(F6A)
Uanis(F4B) = Uanis(F4A)
Uanis(F7A) = Uanis(F7B)
Uanis(F8A) = Uanis(F8B)
Uanis(F9B) = Uanis(F9A)
Uanis(F24A) = Uanis(F24B)
Uanis(F22A) = Uanis(F22B)
Uanis(F23B) = Uanis(F23A)
Uanis(F20A) = Uanis(F20B)
Uanis(F21A) = Uanis(F21B)
Uanis(F19B) = Uanis(F19A)
Uanis(F10B) = Uanis(F10A)
Uanis(F11A) = Uanis(F11B)
Uanis(F12B) = Uanis(F12A)
Uanis(F13B) = Uanis(F13A)
Uanis(F15A) = Uanis(F15B)
Uanis(F14A) = Uanis(F14C)
Uanis(F13A) = Uanis(F13B) = Uanis(F14A) = Uanis(F14C) = Uanis(F15A) =
Uanis(F15B)
Uanis(F11A) = Uanis(F11B) = Uanis(F12A) = Uanis(F12B) = Uanis(F10B) =
Uanis(F10A)
Uanis(F8A) = Uanis(F8B) = Uanis(F7B) = Uanis(F7A) = Uanis(F9B) = Uanis(F9A)
Uanis(F20A) = Uanis(F20B) = Uanis(F21B) = Uanis(F21A) = Uanis(F19B) =
Uanis(F19A)
Uanis(F23A) = Uanis(F23B) = Uanis(F22B) = Uanis(F24A) = Uanis(F24B) =
Uanis(F22A)
Uanis(F6A) = Uanis(F6B)
Uanis(F6B) = Uanis(F6A) = Uanis(F5A) = Uanis(F5B) = Uanis(F4A) = Uanis(F4B)
Uanis(F13C) = Uanis(F13B) = Uanis(F13A) = Uanis(F15C) = Uanis(F15B) =
Uanis(F15A) = Uanis(F14C) = Uanis(F14B) = Uanis(F14A)
3. Others
 Fixed Sof: F4A(0.33333) F4B(0.33333) F4C(0.33333) F5A(0.33333) F5B(0.33333)
 F5C(0.33333) F6A(0.33333) F6B(0.33333) F6C(0.33333) F7A(0.33333) F7B(0.33333)
 F7C(0.33333) F8A(0.33333) F8B(0.33333) F8C(0.33333) F9A(0.33333) F9B(0.33333)
 F9C(0.33333) F10A(0.5) F10B(0.5) F11A(0.5) F11B(0.5) F12A(0.5) F12B(0.5)
 F13A(0.33333) F13B(0.33333) F13C(0.33333) F14A(0.33333) F14B(0.33333)
 F14C(0.33333) F15A(0.33333) F15B(0.33333) F15C(0.33333) F19A(0.5) F19B(0.5)
 F20A(0.5) F20B(0.5) F21A(0.5) F21B(0.5) F22A(0.5) F22B(0.5) F23A(0.5)
 F23B(0.5) F24A(0.5) F24B(0.5)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'