Ni(I)/Ru(II) Model for the Ni-L State of the [NiFe]Hydrogenases: Synthesis, Spectroscopy, and Reactivity.
Chambers, Geoffrey M.; Mitra, Joyee; Rauchfuss, Thomas B.; Stein, Matthias; Inorganic chemistry 53 (2014) 4243–4249; doi:10.1021/ic500389p

data_4337898
_publ_contact_author
; 
Thomas B. Rauchfuss
University of Illinois
A328 CLSL, Box 12-6
600 South Mathews Avenue
Urbana, IL 61801
USA
;
_publ_section_title
;
 Ni(I)/Ru(II) Model for the Ni-L State of the [NiFe]Hydrogenases:
 Synthesis, Spectroscopy, and Reactivity.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4243
_journal_page_last               4249
_journal_paper_doi               10.1021/ic500389p
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C32 H12 B F24, C39 H44 Ni P2 Ru S2'
_chemical_formula_sum            'C71 H56 B F24 Ni P2 Ru S2'
_chemical_formula_weight         1661.81
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                101.1580(10)
_cell_angle_beta                 104.8820(10)
_cell_angle_gamma                93.2380(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7518(12)
_cell_length_b                   16.2382(15)
_cell_length_c                   18.3196(17)
_cell_measurement_reflns_used    7231
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      22.19
_cell_measurement_theta_min      2.21
_cell_volume                     3574.2(6)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V2005/2, SADABS V2008/2, TWINABS V2008/2 
(Bruker, 2005 & 2008) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  bm06was
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39962
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.9229
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1674
_exptl_crystal_id                bm06was
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1, 1, -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.279
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1404
_refine_ls_number_reflns         13393
_refine_ls_number_restraints     4218
_refine_ls_restrained_S_all      1.359
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+6.5267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                9398
_reflns_number_total             13393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500389p_si_002.cif
_cod_data_source_block           bm06was
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4337898--4337899.cif.
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4337898