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_1543713
_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         'C36 H37 O3 P2 Pt S3, B F4'
_chemical_formula_sum            'C36 H37 B F4 O3 P2 Pt S3'
_chemical_formula_weight         957.67
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 101.881(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1695(7)
_cell_length_b                   9.2664(4)
_cell_length_c                   22.3000(9)
_cell_measurement_reflns_used    7028
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.061
_cell_measurement_theta_min      2.865
_cell_volume                     3674.1(3)
_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      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24761
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.439
_diffrn_reflns_theta_min         3.515
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    10.046
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1027 before and 0.0687 after correction.
The Ratio of minimum to maximum transmission is 0.7666.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1896
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.006
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     653
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0472P)^2^+1.8643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4708
_reflns_number_total             6406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01454b2.cif
_cod_data_source_block           cx0591
_cod_depositor_comments
'Adding full bibliography for 1543711--1543714.cif.'
_cod_database_code               1543713
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.520
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P1-C15A \\sim P1-C15
 with sigma of 0.01
 C15A-C16A \\sim C15A-C20A \\sim C16-C15 \\sim C20-C15 \\sim C19-C20 \\sim
C20A-C19A \\sim C18-C19 ~
 C18A-C19A \\sim C17A-C18A \\sim C18-C17 \\sim C17A-C16A \\sim C17-C16
 with sigma of 0.01
 C26-C21 \\sim C26A-C21A \\sim C25A-C26A \\sim C26-C25 \\sim C24-C25 \\sim
C25A-C24A \\sim C24-C23 ~
 C24A-C23A \\sim C22-C23 \\sim C23A-C22A \\sim C21A-C22A \\sim C22-C21
 with sigma of 0.01
 P2-C21 \\sim P2-C21A
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(C15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(2)
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C16A(H16A), C17(H17), C17A(H17A), C18(H18),
 C18A(H18A), C19(H19), C19A(H19A), C20(H20), C20A(H20A), C22(H22), C22A(H22A),
 C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A), C26(H26),
 C26A(H26A), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
;
_shelx_res_checksum              79858
_shelx_hkl_checksum              39741
_olex2_date_sample_data_collection 2015-10-20
_olex2_date_sample_submission    2015-10-20
_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 cx0591
_olex2_submission_special_instructions 'No special instructions were received'