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_4121639
_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
; 
C57 H50 Fe2 O2 P4 S2, B F4, 2 (C H2 Cl2), C5 H12 
;
_chemical_formula_sum            'C61.5 H60 B Cl4 F4 Fe2 O2 P4 S2'
_chemical_formula_weight         1359.40
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6274(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4632(4)
_cell_length_b                   25.4013(8)
_cell_length_c                   17.2705(5)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.20
_cell_volume                     6214.7(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics
; 
SHELXTL v2013-4 (Bruker, 2013), CrystalMaker v2.7.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2013-1 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_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  cm65fasq
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            80258
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.383
_diffrn_reflns_theta_min         1.446
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.8964
_exptl_absorpt_correction_T_min  0.8518
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2792
_exptl_crystal_id                cm65fasq
_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 0 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.232
_platon_squeeze_details
; 
Two dichloromethane and one half of one pentane solvent molecule per 
asymmetric unit were squeezed out.  This accounts for most of the 219 
electrons per void. 
;
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         11355
_refine_ls_number_restraints     391
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0278P)^2^+8.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9170
_reflns_number_total             11355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja501366j_si_002.cif
_cod_data_source_block           cm65fasq
_cod_depositor_comments
'Adding full bibliography for 4121638--4121640.cif.'
_cod_original_formula_sum        'C61.50 H60 B Cl4 F4 Fe2 O2 P4 S2'
_cod_database_code               4121639
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.825
_shelxl_version_number           2013-4
_shelx_res_checksum              51641
_shelx_hkl_checksum              24930