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_1543712
_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_absolute_configuration ad
_chemical_formula_moiety         '2(C44 H46 N4 O3 P S), C H2 Cl2, 2(H2 O)'
_chemical_formula_sum            'C89 H98 Cl2 N8 O8 P2 S2'
_chemical_formula_weight         1604.71
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-03-21 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.831(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   48.8875(19)
_cell_length_b                   6.1721(2)
_cell_length_c                   13.7803(5)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.073
_cell_measurement_theta_min      3.303
_cell_volume                     4037.5(3)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.987
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15230
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.137
_diffrn_reflns_theta_min         3.303
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0655 before and 0.0436 after correction.
The Ratio of minimum to maximum transmission is 0.8440.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       plate
_exptl_crystal_F_000             1696
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 2613 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.019(16)
_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     598
_refine_ls_number_reflns         6673
_refine_ls_number_restraints     251
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+7.7088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.883
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                6308
_reflns_number_total             6673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01454b2.cif
_cod_data_source_block           cx0040a
_cod_depositor_comments
'Adding full bibliography for 1543711--1543714.cif.'
_cod_database_code               1543712
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.803
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 C2, C3, C4, C5, C6, C2A, C3A, C4A, C5A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8, C9, C10, C11, C12, C8A, C9A, C10A, C11A, C12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C2A \\sim C3A \\sim C4A \\sim C5A
\\sim C6A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C8A \\sim C9A \\sim C10A \\sim
C11A \\sim C12A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Others
 Sof(C2A)=Sof(H2AA)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4AA)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4A)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(H6)=FVAR(1)
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=
 Sof(C12A)=Sof(H12A)=1-FVAR(2)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=
 Sof(H12)=FVAR(2)
 Fixed Sof: H1SA(0.5) H1SB(0.5)
5.a Free rotating group:
 O1S(H1SC,H1SD)
5.b Ternary CH refined with riding coordinates:
 N4(H4), C25(H25), C36(H36), C38(H38), C42(H42)
5.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,
 H40B), C41(H41A,H41B), C43(H43A,H43B), C1S(H1SA,H1SB)
5.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C2(H2A), C3(H3), C4(H4A), C5(H5), C6(H6), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C16(H16), C17(H17), C19(H19), C20(H20), C27(H27),
  C28(H28), C30(H30), C31(H31), C33(H33), C2A(H2AA), C3A(H3A), C4A(H4AA),
 C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A)
5.e Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              71288
_shelx_hkl_checksum              54253
_olex2_submission_original_sample_id cx0040a
_olex2_submission_special_instructions 'No special instructions were received'