A concerted two-prong approach to the in situ allosteric regulation of bifunctional catalysis
McGuirk, C. Michael; Mendez-Arroyo, Jose; d'Aquino, Andrea I.; Stern, Charlotte L.; Liu, Yuan; Mirkin, Chad A.; Chem. Sci. 7 (2016) 6674–; doi:10.1039/C6SC01454B

data_1543714
_publ_section_title
;
 A concerted two-prong approach to the in situ allosteric regulation of
 bifunctional catalysis
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6674
_journal_paper_doi               10.1039/C6SC01454B
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C32 H12 B F24, 2(C2.5 H3 N0.5)'
_chemical_formula_sum            'C37 H18 B F24 N'
_chemical_formula_weight         943.33
_chemical_name_systematic        'pyridinium BArF'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-21 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                79.884(3)
_cell_angle_beta                 76.218(3)
_cell_angle_gamma                63.750(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3832(6)
_cell_length_b                   12.7027(6)
_cell_length_c                   13.6428(6)
_cell_measurement_reflns_used    8509
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.560
_cell_measurement_theta_min      3.082
_cell_volume                     1863.19(16)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_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_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27044
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         1.793
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0640 before and 0.0372 after correction.
The Ratio of minimum to maximum transmission is 0.9342.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.108
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         9629
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0860P)^2^+1.9010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6936
_reflns_number_total             9629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01454b2.cif
_cod_data_source_block           cx0613
_cod_depositor_comments
'Adding full bibliography for 1543711--1543714.cif.'
_cod_original_cell_volume        1863.20(16)
_cod_database_code               1543714
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Shared sites
{C38, N1}
{C35, N2}
{C33, N3}
3. Restrained distances
 C34-H34
 0.95 with sigma of 0.02
 F14A-F13A \\sim F14-F13
 with sigma of 0.01
 F15-C23 \\sim F14A-C23 \\sim F14-C23 \\sim F13A-C23 \\sim F13-C23 \\sim
F15A-C23
 with sigma of 0.01
4. Rigid bond restraints
 F13, F13A, F14, F14A, F15, F15A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
F13 \\sim F13A \\sim F14 \\sim F14A \\sim F15 \\sim F15A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.001
Uanis(C38) = Uanis(N1)
Uanis(C35) = Uanis(N2)
Uanis(C33) = Uanis(N3)
6. Others
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Fixed Sof: N1(0.5) H1(0.5) H36(0.5) H36A(0.5) H37(0.5) H37A(0.5) C38(0.5)
 H38(0.5) N2(0.25) H2A(0.25) N3(0.25) H3(0.25) C33(0.75) H33(0.75) C35(0.75)
 H35(0.75)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C10(H10), C12(H12), C14(H14), C17(H17), C19(H19),
 C21(H21), C26(H26), C28(H28), C30(H30), N1(H1), C36(H36), C36(H36A), C37(H37),
 C37(H37A), C38(H38), N2(H2A), N3(H3), C33(H33), C35(H35)
;
_shelx_res_checksum              44333
_shelx_hkl_checksum              25756
_olex2_date_sample_data_collection 2015-11-11
_olex2_date_sample_submission    2015-11-11
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx0613
_olex2_submission_special_instructions 'No special instructions were received'