New Reactions of Terminal Hydrides on a Diiron Dithiolate.
Wang, Wenguang; Rauchfuss, Thomas B.; Zhu, Lingyang; Zampella, Giuseppe; Journal of the American Chemical Society 136 (2014) 5773–; doi:10.1021/ja501366j

data_4121640
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 New Reactions of Terminal Hydrides on a Diiron Dithiolate.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5773
_journal_paper_doi               10.1021/ja501366j
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'2(C34 H32 Fe2 N O3 P2 S2), 2(F6 P), 1.5(C H2 Cl2)'
_chemical_formula_sum            'C69.5 H67 Cl3 F12 Fe4 N2 O6 P6 S4'
_chemical_formula_weight         1898.06
_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
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.767(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5145(16)
_cell_length_b                   16.1220(11)
_cell_length_c                   24.2383(15)
_cell_measurement_reflns_used    2966
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.00
_cell_measurement_theta_min      2.14
_cell_volume                     8130.7(10)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, 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      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ba00nasq
_diffrn_reflns_av_R_equivalents  0.1949
_diffrn_reflns_av_sigmaI/netI    0.1356
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            130178
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.9452
_exptl_absorpt_correction_T_min  0.8445
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3852
_exptl_crystal_id                ba00nasq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-2 0 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.068
_platon_squeeze_details
; 
The electron count from the "squeeze" model 
converged in good agreement with two methylene chloride molecules in two 
holes. This corresponds to half of a methylene cholride molecule in the 
assymetric unit, which is predicted by the complete refinement. 
;
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         14902
_refine_ls_number_restraints     530
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1440
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                8403
_reflns_number_total             14902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja501366j_si_002.cif
_cod_data_source_block           ba00nasq
_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 4121638--4121640.cif.
;
_cod_original_cell_volume        8130.7(9)
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_original_formula_sum        'C69.50 H67 Cl3 F12 Fe4 N2 O6 P6 S4'
_cod_database_code               4121640