Robust Affinity Standards for Cu(I) Biochemistry
Pritha Bagchi; M. Thomas Morgan; John Bacsa; Christoph J. Fahrni; Journal of the American Chemical Society 135 (2013) 18549–18559; doi:10.1021/ja408827d

data_4121279
_publ_contact_author_address
;
School of Chemistry and Biochemistry, 
Petit Institute for Bioengineering and Bioscience, 
Georgia Institute of Technology, 
901 Atlantic Drive, Atlanta, 
GA 30332, U.S.A.
;
_publ_contact_author_email       fahrni@chemistry.gatech.edu
_publ_contact_author_name        'Christoph J. Fahrni'
_publ_section_title
;
 Robust Affinity Standards for Cu(I) Biochemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18549
_journal_page_last               18559
_journal_paper_doi               10.1021/ja408827d
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C16 H32 O4 S4'
_chemical_formula_sum            'C16 H32 O4 S4'
_chemical_formula_weight         416.65
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-07-07
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                100.741(2)
_cell_angle_beta                 107.2010(10)
_cell_angle_gamma                97.413(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5948(9)
_cell_length_b                   9.6412(9)
_cell_length_c                   12.1268(12)
_cell_measurement_reflns_used    4864
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      31.051
_cell_measurement_theta_min      2.266
_cell_volume                     1032.38(17)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 diffractometer with APEX2 detector'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7622
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.216
_diffrn_reflns_theta_min         1.809
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.559773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0922 before and 0.0496 after correction.
 The Ratio of minimum to maximum transmission is 0.75.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0925 before and 0.0476 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 17303 reflections, Rint = 0.1021
 (11141 with I > 3sig(I), Rint = 0.0976)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.774
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.196
_refine_diff_density_max         1.736
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         7622
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+3.5031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2297
_refine_ls_wR_factor_ref         0.2354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6791
_reflns_number_total             7622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja408827d_si_002_4.cif
_cod_data_source_block           16
_cod_database_code               4121279
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups
2. Restrained distances
 C5A-C4A = C5B-C4B
 1.52 with sigma of 0.01
 H4-H1_$1
 -2.045 with sigma of 0.02
 S2B-C3 \\sim S2A-C3
 with sigma of 0.005
 S3B-C7 \\sim S3A-C7
 with sigma of 0.005
 S3A-C7 \\sim S3B-C7
 with sigma of 0.004
 S2A-C4A \\sim S2B-C4B
 with sigma of 0.004
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(S3B) \\sim Ueq, Uanis(S3A) \\sim Ueq, 
Uanis(C6B) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5B) \\sim Ueq, 
Uanis(C5A) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C4A) \\sim Ueq, 
Uanis(S2B) \\sim Ueq, Uanis(S2A) \\sim Ueq: with sigma of 0.002 and 
sigma for terminal atoms of 0.004
Uanis(S2A) = Uanis(S2B)
Uanis(C4A) = Uanis(C4B)
Uanis(C5A) = Uanis(C5B)
Uanis(C6A) = Uanis(C6B)
Uanis(S3A) = Uanis(S3B)
4. others
 Fixed Sof: S2A(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5)
 C6A(0.5) H6AA(0.5) H6AB(0.5) S3A(0.5) S2B(0.5) C4B(0.5) H4BA(0.5) H4BB(0.5)
 C5B(0.5) H5BA(0.5) H5BB(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) S3B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7(H7A,H7B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B)
5.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O4(H4)
;
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.709
_shelxl_version_number           2013-4