Borane-Protected Cyanides as Surrogates of H-Bonded Cyanides in [FeFe]-Hydrogenase Active Site Models.
Manor, Brian C.; Ringenberg, Mark R.; Rauchfuss, Thomas B.; Inorganic chemistry 53 (2014) 7241–7247; doi:10.1021/ic500470z

data_4340354
_publ_contact_author
; 
Thomas B. Rauchfuss 
University of Illinois 
Department of Chemistry 
A328 Chemical & Life Sciences Lab 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Borane-Protected Cyanides as Surrogates of H-Bonded Cyanides in
 [FeFe]-Hydrogenase Active Site Models.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7241
_journal_page_last               7247
_journal_paper_doi               10.1021/ic500470z
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
; 
C45 H6 B2 F30 Fe2 N2 O4 S2, 2(C8 H20 N), C4 H8 O 
;
_chemical_formula_sum            'C65 H54 B2 F30 Fe2 N4 O5 S2'
_chemical_formula_weight         1738.56
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90.00
_cell_angle_beta                 106.507(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.194(2)
_cell_length_b                   20.4776(13)
_cell_length_c                   17.1835(10)
_cell_measurement_reflns_used    7094
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      19.43
_cell_measurement_theta_min      2.34
_cell_volume                     14235.2(14)
_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 V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_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      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Siemens Platform/ApexII CCD'
_diffrn_measurement_device_type  'CCD area detector'
_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  ba75jas
_diffrn_reflns_av_R_equivalents  0.1416
_diffrn_reflns_av_sigmaI/netI    0.0932
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            102155
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.9652
_exptl_absorpt_correction_T_min  0.8289
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7008
_exptl_crystal_id                ba75jas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-5 0 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.582
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1246
_refine_ls_number_reflns         13119
_refine_ls_number_restraints     998
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+14.8408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                7159
_reflns_number_total             13119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500470z_si_002.cif
_cod_data_source_block           ba75jas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/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 4340354.cif.
;
_cod_original_cell_volume        14235.0(15)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4340354