New Class of Diiron Dithiolates Related to the Fe-Only Hydrogenase Active Site: Synthesis and Characterization of [Fe2(SR)2(CNMe)7]2+
Joshua D. Lawrence; Thomas B. Rauchfuss; Scott R. Wilson; Inorganic Chemistry 41 (2002) 6193–6195; doi:10.1021/ic025919t

data_4318960
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 New Class of Diiron Dithiolates Related to the Fe-Only Hydrogenase Active
 Site: Synthesis and Characterization of [Fe2(SR)2(CNMe)7]2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6193
_journal_page_last               6195
_journal_paper_doi               10.1021/ic025919t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C17 H27 Fe2 N7 S2 2+, 2(F6 P 1-), C H2 Cl2'
_chemical_formula_sum            'C18 H29 Cl2 F12 Fe2 N7 P2 S2'
_chemical_formula_weight         880.14
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2002-04-17   text and data added, jdl 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.658(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.984(3)
_cell_length_b                   15.877(4)
_cell_length_c                   22.094(6)
_cell_measurement_reflns_used    889
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.78
_cell_measurement_theta_min      2.57
_cell_volume                     3452.6(16)
_computing_cell_refinement       'SAINT V6 (Bruker, 2001)'
_computing_data_collection       'SMART V5 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6 (Bruker, 2000)'
_computing_publication_material  'CIFTAB (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL V6 (Bruker, 2000)'
_computing_structure_solution    'SHELXTL V6 (Bruker, 2000)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \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  p25rfas
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1753
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24185
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        5.4
_diffrn_standards_interval_time  402
_diffrn_standards_number         175
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.95036
_exptl_absorpt_correction_T_min  0.75642
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2000)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platy
_exptl_crystal_F_000             1768
_exptl_crystal_id                p25rfas
_exptl_crystal_preparation
; 
All crystals examined suffered from nonmerohedral twinning defined 
by a pseudo-twofold axis normal to the b,c-plane.  The primary and 
secondary oreintations were integrated separately. All reflections 
with complete or no overlap from both sets were combined and refined 
against a batch scale factor.  The data crystal was mounted using oil 
(Parantone-N, Exxon) to a thin glass fiber with the (0 0 1) 
scattering planes of the primary orientation and (0 0 -1) planes of 
the secondary orientation roughly normal to the spindle axis.  Faces 
for the primary orientation are listed herein. 
;
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         23773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1649
_refine_ls_R_factor_gt           0.0709
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1870
_reflns_number_gt                11263
_reflns_number_total             23773
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025919t-3_s1_2.cif
_cod_data_source_block           p25rfas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3452.7(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4318960