Substrate Binding Preferences and pKa Determinations of a Nitrile Hydratase Model Complex: Variable Solvent Coordination to [(bmmp-TASN)Fe]OTf
Martin G. O'Toole; Brian Bennett; Mark S. Mashuta; Craig A. Grapperhaus; Inorganic Chemistry 48 (2009) 2300–2308; doi:10.1021/ic802180d

data_4301618
_publ_contact_author_address
;
Department of Chemistry
University of Louisville
2320 So. Brook St.
Louisville
KY 40292
USA
;
_publ_contact_author_email       craig.grapperhaus@louisville.edu
_publ_contact_author_fax         502-852-8149
_publ_contact_author_name        'Craig A. Grapperhaus'
_publ_contact_author_phone       502-852-5932
_publ_section_title
;
Substrate Binding Preferences and pKa Determinations of a Nitrile Hydratase
Model Complex: Variable Solvent Coordination to [(bmmp-TASN)Fe]OTf
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2300
_journal_page_last               2308
_journal_paper_doi               10.1021/ic802180d
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
;
C28 H57 Fe2 N4 O S6, C F3 O3 S, 0.75(C H4 O) 
;
_chemical_formula_sum            'C29.75 H60 F3 Fe2 N4 O4.75 S7'
_chemical_formula_weight         942.94
_chemical_name_common
; 
 
[((N,N'-4,7-bis-(2'-methyl-2'-mercatopropyl)
-1-thia-4,7-diazacyclononane)Fe)2OH]OTf 
;
_chemical_name_systematic
; 
 
[((N,N'-4,7-bis-(2'-methyl-2'-mercatopropyl)
-1-thia-4,7-diazacyclononane)Fe)2OH]OTf 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             Aug_13_2008
_audit_creation_method           SHELXL-97
_audit_update_record
;
Aug_22_2008 text added by Mark S. Mashuta
Sept_11_2008 text added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.172(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.472(6)
_cell_length_b                   10.629(4)
_cell_length_c                   25.894(13)
_cell_measurement_reflns_used    6779
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.64
_cell_volume                     4241(3)
_computing_cell_refinement       'SAINT 6.36 (Bruker, 2002)'
_computing_data_collection       'SMART 5.628 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36 (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 6.14 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.14 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            18021
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction was based upon symmetry equivalent and
repeated intensity measurements using the program SADABS
(Sheldrick, 2001).
;
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       trapezoid-prism
_exptl_crystal_F_000             1982
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.030(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9283
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.00
_refine_ls_shift/su_mean         0.00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+1.9716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                8773
_reflns_number_total             9283
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic802180d_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               4301618