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_4121278
_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         'F6 P, C16 H32 Cu O4 S4, C2 H6 O'
_chemical_formula_sum            'C18 H38 Cu F6 O5 P S4'
_chemical_formula_weight         671.28
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-02-27
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                71.5710(10)
_cell_angle_beta                 77.6760(10)
_cell_angle_gamma                78.8850(10)
_cell_formula_units_Z            4
_cell_length_a                   13.4862(5)
_cell_length_b                   13.6947(4)
_cell_length_c                   15.8096(5)
_cell_measurement_reflns_used    9668
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      40.617
_cell_measurement_theta_min      2.377
_cell_volume                     2681.44(15)
_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 0.995
_diffrn_measured_fraction_theta_max 0.972
_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_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            110771
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        35.000
_diffrn_reflns_theta_max         40.718
_diffrn_reflns_theta_min         1.376
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.6912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0617 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.7019.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.712
_exptl_crystal_size_mid          0.356
_exptl_crystal_size_min          0.184
_refine_diff_density_max         1.974
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         33773
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0543P)^2^+0.8792P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28769
_reflns_number_total             33773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja408827d_si_002_3.cif
_cod_data_source_block           12
_cod_original_cell_volume        2681.45(15)
_cod_database_code               4121278
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H10A,H10B} of C10, {H14A,H14B} of C14, H1 of O1, H4 of O4, {H28A,H28B} of
  C28, H3 of O3, {H29A,H29B} of C29, {H30A,H30B} of C30, {H31A,H31B} of C31,
  {H32A,H32B} of C32, H5 of O5, H6 of O6, H7 of O7, H8 of O8, {H11A,H11B} of
  C11, {H27A,H27B} of C27, {H26A,H26B} of C26, {H25A,H25B} of C25, {H13A,H13B}
  of C13, {H23A,H23B} of C23, {H19A,H19B} of C19, {H17A,H17B} of C17, {H9A,H9B}
  of C9, {H4A,H4B} of C4, H2 of O2, {H20C,H20D} of C20', H9 of O9, {H22C,H22D}
  of C22', {H21A,H21B} of C21, {H20A,H20B} of C20, {H22A,H22B} of C22, {H21C,
  H21D} of C21', {H3A,H3B} of C3, {H6A,H6B} of C6, {H15A,H15B} of C15, {H7A,
  H7B} of C7, {H5A,H5B} of C5, {H1A,H1B} of C1, {H12A,H12B} of C12, {H16A,H16B}
  of C16, {H33A,H33B} of C33, H10 of O10, {H35A,H35B} of C35
 At 1.5 times of:
  {H36A,H36B,H36C} of C36, {H34A,H34B,H34C} of C34
2. Restrained distances
 C21-C20' ~ C21'-C20'
 with sigma of 0.005
 C22'-C21 ~ C22'-C21'
 with sigma of 0.005
 S6-C20 ~ S6-C20'
 with sigma of 0.005
 S7-C22' ~ S7-C22
 with sigma of 0.005
 P2B-F9B ~ P2B-F7B ~ P2B-F11B ~ P2B-F12B ~ P2B-F10B ~ P2B-F8B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uiso(C20) = Uiso(C20')
Uiso(C22) = Uiso(C22')
Uanis(P1A) = Uanis(P1B)
Uanis(F1A) = Uanis(F1B)
Uanis(F2A) = Uanis(F2B)
Uanis(F3A) = Uanis(F3B)
Uanis(F4A) = Uanis(F4B)
Uanis(F5A) = Uanis(F5B)
Uanis(F6A) = Uanis(F6B)
Uanis(P2A) = Uanis(P2B)
Uanis(F9A) = Uanis(F9B)
Uanis(F11A) = Uanis(F11B)
Uanis(F8A) = Uanis(F8B)
Uanis(F10A) = Uanis(F10B)
Uanis(F7A) = Uanis(F7B)
Uanis(F12A) = Uanis(F12B)
4. Same fragment restrains
{P2B, F7B, F8B, F9B, F10B, F11B, F12B}
as
{P2A, F7A, F8A, F9A, F10A, F11A, F12A}
{C20', C21', C22'}
as
{C20, C21, C22}
{P1B, F1B, F2B, F3B, F4B, F5B, F6B}
as
{P1A, F1A, F2A, F3A, F4A, F5A, F6A}
5. others
 Sof(P1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-Sof(F1A)=1-
 Sof(F1A)=1-Sof(F1A)=1-Sof(F1A)=1-Sof(F1A)=1-Sof(F1A)=1-Sof(F1A)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=1-Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)=1-
 Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)
 Sof(P2A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-Sof(F7A)=
 1-Sof(F7A)=1-Sof(F7A)=1-Sof(F7A)=1-Sof(F7A)=1-Sof(F7A)=1-Sof(F7A)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B), C4(H4A,H4B), C14(H14A,H14B), C10(H10A,H10B),
 C11(H11A,H11B), C13(H13A,H13B), C9(H9A,H9B), C3(H3A,H3B), C6(H6A,H6B),
 C15(H15A,H15B), C7(H7A,H7B), C5(H5A,H5B), C1(H1A,H1B), C12(H12A,H12B),
 C16(H16A,H16B), C33(H33A,H33B), C35(H35A,H35B), C20(H20A,H20B), C21(H21A,H21B),
  C22(H22A,H22B), C20'(H20C,H20D), C21'(H21C,H21D), C22'(H22C,H22D)
6.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
6.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6), O7(H7), O8(H8), O2(H2), O4(H4), O1(H1), O3(H3), O10(H10),
 O9(H9)
;
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.468
_shelxl_version_number           2012-9