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_4121277
_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
'C18 H36 Cu N O9 S6, F6 P -, 3(Na +), 7.5(H2 O)'
_chemical_formula_sum            'C18 H51 Cu F6 N Na3 O16.5 P S6'
_chemical_formula_weight         1015.43
_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   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-07-02
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                91.273(2)
_cell_angle_beta                 98.023(2)
_cell_angle_gamma                119.384(2)
_cell_formula_units_Z            4
_cell_length_a                   11.8551(17)
_cell_length_b                   11.9311(17)
_cell_length_c                   32.214(5)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.08
_cell_measurement_theta_min      2.18
_cell_volume                     3909.7(10)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0266
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            50063
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.106
_diffrn_reflns_theta_min         1.284
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.8602
_exptl_absorpt_correction_T_min  0.6223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0547 before and 0.0411 after correction.
The Ratio of minimum to maximum transmission is 0.7234.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       prism
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.783
_exptl_crystal_size_mid          0.451
_exptl_crystal_size_min          0.316
_refine_diff_density_max         1.934
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1277
_refine_ls_number_reflns         25380
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      6.452
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0690P)^2^+3.0344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19582
_reflns_number_total             25380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja408827d_si_002_2.cif
_cod_data_source_block           14a
_cod_depositor_comments
;

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 H102 Cu2 F12 N2 Na6 O33 P2 S12'
_cod_original_formula_weight         2030.87
_cod_original_formula_moiety
'C36 H96 Cu2 N2 Na6 O30 S12, 2(F6 P), 3(H2 O)'
_cod_original_formula_units_Z            2
_cod_database_code               4121277
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O15W-H15A = O15W-H15B
 0.99 with sigma of 0.01
 H15B-H15A
 1.585 with sigma of 0.01
 O5W-H5WA = O5W-H5WB
 0.99 with sigma of 0.01
 H5WA-H5WB
 1.585 with sigma of 0.01
 O13W-H13B = O13W-H13A
 0.99 with sigma of 0.01
 H13B-H13A
 1.585 with sigma of 0.01
 O2W-H2WB = O2W-H2WA
 0.99 with sigma of 0.01
 H2WB-H2WA
 1.585 with sigma of 0.01
 O12W-H12A = O12W-H12B
 0.99 with sigma of 0.01
 H12A-H12B
 1.585 with sigma of 0.01
 O14W-H14E = O14W-H14F
 0.99 with sigma of 0.01
 H14F-H14E
 1.585 with sigma of 0.01
 O7W-H7WB = O7W-H7WA
 0.99 with sigma of 0.01
 H7WB-H7WA
 1.585 with sigma of 0.01
 O1W-H1WA = O1W-H1WB
 0.99 with sigma of 0.01
 H1WB-H1WA
 1.585 with sigma of 0.01
 O11W-H11B = O11W-H11A
 0.99 with sigma of 0.01
 H11B-H11A
 1.585 with sigma of 0.01
 O4W-H4WA
 0.99 with sigma of 0.01
 O4W-H4WB
 0.99 with sigma of 0.01
 H4WA-H4WB
 1.59 with sigma of 0.01
 O7B-H4WB
 1.92 with sigma of 0.01
 O6-H4WA
 1.77 with sigma of 0.01
 O3W-H3WA
 0.99 with sigma of 0.01
 H3WA-Na2
 2.75 with sigma of 0.01
 O3W-H3WA
 0.99 with sigma of 0.01
 O6W-H6WB = O6W-H6WA
 0.99 with sigma of 0.01
 H6WA-H6WB
 1.585 with sigma of 0.01
 O3W-H3WB
 0.99 with sigma of 0.01
 H3WA-H3WB
 1.585 with sigma of 0.01
 Na1-H3WB
 2.7 with sigma of 0.01
 O2B-H6WA
 1.733 with sigma of 0.02
 H3WB_$4-H3WB_$3
 1.99 with sigma of 0.01
 O8W-H8WA
 0.985 with sigma of 0.01
 O8W-H8WB
 0.985 with sigma of 0.01
 H8WB-H8WA
 1.555 with sigma of 0.01
 O10W-H10B = O10W-H10A
 0.99 with sigma of 0.01
 H10B-H10A
 1.585 with sigma of 0.01
 O9W-H9WA = O9W-H9WB
 0.985 with sigma of 0.01
 H9WA-H9WB
 1.555 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(H3WB) = Uiso(H3WA)
Uiso(H9WA) = Uiso(H9WB)
4. others
 Fixed Uiso: H6WA(0.02018) H6WB(0.02018) H9WA(0.02296) H9WB(0.02296)
;
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.494
_shelxl_version_number           2013-4