Hydrogen Production Catalyzed by Bidirectional, Biomimetic Models of the [FeFe]-Hydrogenase Active Site.
Lansing, James C.; Camara, James M.; Gray, Danielle E.; Rauchfuss, Thomas B.; Organometallics 33 (2014) 5897–5906; doi:10.1021/om5004013

data_4083862
_publ_section_title
;
 Hydrogen Production Catalyzed by Bidirectional, Biomimetic Models of the
 [FeFe]-Hydrogenase Active Site.
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5897
_journal_page_last               5906
_journal_paper_doi               10.1021/om5004013
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety
; 
(C62 H72 Fe3 N O3 P3 S2), 1/3(C4 H10 O) 
;
_chemical_formula_sum            'C63.33 H75.33 Fe3 N O3.33 P3 S2'
_chemical_formula_weight         1228.49
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   37.6828(18)
_cell_length_b                   37.6828(18)
_cell_length_c                   22.160(2)
_cell_measurement_reflns_used    9188
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      22.66
_cell_measurement_theta_min      2.16
_cell_volume                     27251(3)
_computing_cell_refinement       'SAINT V7.68A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2010.11-3 (Bruker, 2010)'
_computing_data_reduction
; 
SAINT V7.68A, XPREP V6.12, SADABS V2008/1, TWINABS V2008/2 
(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  'SHELX-2013v9 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013v9 (Sheldrick, 2013)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  bm43vasq
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49220
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.362
_diffrn_reflns_theta_min         1.550
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.9196
_exptl_absorpt_correction_T_min  0.7896
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             11592
_exptl_crystal_id                bm43vasq
_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, -4, -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.474
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.108
_platon_squeeze_details
; 
A total of 295 electrons were squeezed out of the unit cell.  This accounts 
for the 6 diethylether molecules that were modeled in the unit cell prior 
to sqeezing the data.  Some of the voids from which the electron density 
was squeezed are broken into smaller sizes (volume of 48; electron count 
of 8) due to the disorder in the molecule.  This is why there are three large 
voids and many smaller voids. 
;
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         11085
_refine_ls_number_restraints     1628
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0638P)^2^+5.9390P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7016
_reflns_number_total             11085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5004013_si_002.cif
_cod_data_source_block           Molecule1
_cod_depositor_comments
'Adding full bibliography for 4083859--4083862.cif.'
_cod_original_cell_volume        27252(4)
_cod_database_code               4083862
_shelx_estimated_absorpt_t_min   0.674
_shelx_estimated_absorpt_t_max   0.909
_shelxl_version_number           2012-9
_shelx_res_checksum              17521
_shelx_hkl_checksum              3431