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_1543711
_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         'C16 H18 O3 P S2, Na, 1.5(H2 O)'
_chemical_formula_sum            'C16 H21 Na O4.5 P S2'
_chemical_formula_weight         403.41
_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             2016-02-12
_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                 104.918(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.3940(10)
_cell_length_b                   5.6190(2)
_cell_length_c                   25.1528(10)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.103
_cell_measurement_theta_min      3.568
_cell_volume                     4014.3(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      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27769
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.207
_diffrn_reflns_theta_min         1.555
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.543
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0949 before and 0.0519 after correction.
The Ratio of minimum to maximum transmission is 0.7757.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       needle
_exptl_crystal_F_000             1688
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.746
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      6.255
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0730P)^2^+8.0227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6102
_reflns_number_total             6828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01454b2.cif
_cod_data_source_block           cx0580
_cod_depositor_comments
'Adding full bibliography for 1543711--1543714.cif.'
_cod_original_formula_sum        'C16 H21 Na O4.50 P S2'
_cod_database_code               1543711
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.374
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1S-H1SB = O1S-H1SA
 0.87 with sigma of 0.01
 O2S-H2SA \\sim O2S-H2SB
 with sigma of 0.01
 H2SA-H2SB \\sim H1SA-H1SB \\sim H3SA-H3SB
 with sigma of 0.001
 O2S-H2SA \\sim O2S-H2SB \\sim O1S-H1SA \\sim O1S-H1SB \\sim O3S-H3SA \\sim
O3S-H3SB
 with sigma of 0.01
 S2A-O2A \\sim S2A-O2B \\sim S2A-O1A \\sim S2A-O1B \\sim S2A-O3A \\sim S2A-O3B
 with sigma of 0.01
3. Rigid bond restraints
 O3B, O3A, O1B, O1A, O2B, O2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3B \\sim O3A \\sim O1B \\sim O1A \\sim O2B \\sim O2A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O1B)=Sof(O3B)=Sof(O2B)=1-FVAR(1)
 Sof(O1A)=Sof(O2A)=Sof(O3A)=FVAR(1)
6.a Free rotating group:
 H1SA(H1SB), H3SA(H3SB)
6.b Secondary CH2 refined with riding coordinates:
 C12(H12C,H12D), C14(H14C,H14D), C15(H15C,H15D), C16(H16A,H16B), C12A(H12A,
 H12B), C13A(H13A,H13B), C14A(H14A,H14B), C15A(H15A,H15B)
6.c Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10),
 C11(H11), C13(H13), C2A(H2A), C3A(H3A), C4(H4), C4A(H4A), C5A(H5A), C6A(H6A),
 C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A)
;
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  As the exact
solvent content is not known, only the atoms used in the refinement model are
reported in the formula here.

Total solvent accessible volume / cell = 340.4 Ang^3^ [8.5%]
Total electron count / cell = 78.5
;
_shelx_res_checksum              22613
_shelx_hkl_checksum              2356
_olex2_date_sample_data_collection 2015-10-12
_olex2_date_sample_submission    2015-10-09
_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 cx0580
_olex2_submission_special_instructions 'No special instructions were received'