#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:00:37 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178832 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/86/4108672.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4108672
loop_
_publ_author_name
'Yanhui Chen'
'Yuhan Zhou'
'Pingping Chen'
'Yinsong Tao'
'Yang Li'
'Jingping Qu'
_publ_section_title
;
 Nitrogenase Model Complexes [Cp*Fe(μ-SR1)2(μ-η2-R2N=NH)FeCp*] (R1= Me,
 Et; R2= Me, Ph; Cp* = η5-C5Me5): Synthesis, Structure, and Catalytic N-N
 Bond Cleavage of Hydrazines on Diiron Centers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15250
_journal_page_last               15251
_journal_paper_doi               10.1021/ja805025w
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C25 H44 Fe2 N2 S2'
_chemical_formula_weight         548.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.4890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6825(2)
_cell_length_b                   20.3381(4)
_cell_length_c                   8.7589(2)
_cell_measurement_reflns_used    4087
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      30.77
_cell_measurement_theta_min      2.67
_cell_volume                     1346.32(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9127
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prim
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0731
_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/[σ²(Fo²)+(0.0630P)²+7.9049P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.1780
_reflns_number_gt                2446
_reflns_number_total             2678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805025w_si_004.cif
_cod_data_source_block           ds1
_cod_database_code               4108672
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.40686(10) 0.17214(3) 0.33767(9) 0.0383(3) Uani 1 1 d .
S2 S 0.5978(3) 0.2500 0.5213(2) 0.0398(4) Uani 1 2 d S
S3 S 0.2118(3) 0.2500 0.3271(2) 0.0398(4) Uani 1 2 d S
N1 N 0.4098(6) 0.2178(2) 0.1555(5) 0.0446(10) Uani 1 1 d .
C1 C 0.410(3) 0.1170(5) 0.6734(18) 0.268(14) Uani 1 1 d .
H1A H 0.4189 0.0773 0.7363 0.402 Uiso 1 1 calc R
H1B H 0.2995 0.1383 0.6416 0.402 Uiso 1 1 calc R
H1C H 0.5058 0.1459 0.7465 0.402 Uiso 1 1 calc R
C2 C 0.0662(15) 0.0915(5) 0.286(3) 0.191(9) Uani 1 1 d .
H2A H 0.0304 0.0473 0.2905 0.287 Uiso 1 1 calc R
H2B H -0.0054 0.1087 0.1694 0.287 Uiso 1 1 calc R
H2C H 0.0516 0.1183 0.3678 0.287 Uiso 1 1 calc R
C3 C 0.2151(17) 0.0627(5) 0.0286(13) 0.123(4) Uani 1 1 d .
H3A H 0.2046 0.0159 0.0143 0.184 Uiso 1 1 calc R
H3B H 0.2688 0.0802 -0.0359 0.184 Uiso 1 1 calc R
H3C H 0.0997 0.0817 -0.0148 0.184 Uiso 1 1 calc R
C4 C 0.6328(16) 0.0644(5) 0.250(2) 0.152(6) Uani 1 1 d .
H4A H 0.6568 0.0180 0.2614 0.228 Uiso 1 1 calc R
H4B H 0.7415 0.0882 0.3159 0.228 Uiso 1 1 calc R
H4C H 0.5797 0.0766 0.1282 0.228 Uiso 1 1 calc R
C5 C 0.7526(16) 0.0935(5) 0.6335(18) 0.179(8) Uani 1 1 d .
H5A H 0.7891 0.0494 0.6739 0.268 Uiso 1 1 calc R
H5B H 0.7604 0.1199 0.7280 0.268 Uiso 1 1 calc R
H5C H 0.8282 0.1116 0.5930 0.268 Uiso 1 1 calc R
C6 C 0.5607(11) 0.0930(4) 0.4824(12) 0.074(2) Uani 1 1 d .
C7 C 0.4187(17) 0.1011(3) 0.5122(11) 0.094(3) Uani 1 1 d .
C8 C 0.2562(10) 0.0919(3) 0.3308(13) 0.074(2) Uani 1 1 d .
C9 C 0.3304(10) 0.0795(3) 0.2237(9) 0.0585(16) Uani 1 1 d .
C10 C 0.5077(11) 0.0807(3) 0.3177(13) 0.074(2) Uani 1 1 d .
C11 C 0.9679(15) 0.2500 0.6452(16) 0.101(5) Uani 1 2 d S
H11A H 1.0599 0.2500 0.6145 0.152 Uiso 1 2 d SR
H11B H 0.9785 0.2885 0.7130 0.152 Uiso 0.50 1 d PR
C12 C 0.7920(11) 0.2500 0.4793(10) 0.051(2) Uani 1 2 d S
H12A H 0.7839 0.2881 0.4111 0.061 Uiso 1 1 d R
C13 C -0.1552(13) 0.2500 0.0769(14) 0.076(3) Uani 1 2 d S
H13A H -0.2444 0.2500 -0.0447 0.114 Uiso 1 2 d SR
H13B H -0.1681 0.2115 0.1329 0.114 Uiso 1 1 d R
C14 C 0.0261(11) 0.2500 0.0969(10) 0.055(2) Uani 1 2 d S
H14A H 0.0366 0.2119 0.0381 0.066 Uiso 1 1 d R
C15 C 0.4106(15) 0.1978(6) -0.0049(14) 0.047(3) Uani 0.50 1 d P
H15A H 0.4126 0.2362 -0.0677 0.071 Uiso 0.50 1 calc PR
H15B H 0.3061 0.1726 -0.0774 0.071 Uiso 0.50 1 calc PR
H15C H 0.5135 0.1715 0.0253 0.071 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Fe1 C7 165.4(3) . .
N1 Fe1 C8 130.1(3) . .
C7 Fe1 C8 43.4(4) . .
N1 Fe1 C6 129.5(3) . .
C7 Fe1 C6 39.2(4) . .
C8 Fe1 C6 67.4(3) . .
N1 Fe1 C9 100.2(2) . .
C7 Fe1 C9 67.1(3) . .
C8 Fe1 C9 39.3(3) . .
C6 Fe1 C9 63.2(3) . .
N1 Fe1 C10 100.9(3) . .
C7 Fe1 C10 64.7(3) . .
C8 Fe1 C10 65.4(3) . .
C6 Fe1 C10 36.4(3) . .
C9 Fe1 C10 37.4(3) . .
N1 Fe1 S2 86.91(14) . .
C7 Fe1 S2 102.0(3) . .
C8 Fe1 S2 142.6(3) . .
C6 Fe1 S2 94.7(2) . .
C9 Fe1 S2 156.1(2) . .
C10 Fe1 S2 119.0(2) . .
N1 Fe1 S3 86.65(15) . .
C7 Fe1 S3 106.3(3) . .
C8 Fe1 S3 95.72(19) . .
C6 Fe1 S3 143.3(3) . .
C9 Fe1 S3 123.5(2) . .
C10 Fe1 S3 160.2(2) . .
S2 Fe1 S3 79.32(6) . .
C12 S2 Fe1 105.66(18) . .
C12 S2 Fe1 105.66(18) . 4_565
Fe1 S2 Fe1 87.78(7) . 4_565
C14 S3 Fe1 105.9(2) . 4_565
C14 S3 Fe1 105.9(2) . .
Fe1 S3 Fe1 87.65(8) 4_565 .
N1 N1 C15 106.1(5) 4_565 .
N1 N1 Fe1 120.03(14) 4_565 .
C15 N1 Fe1 133.8(6) . .
C7 C1 H1A 109.5 . .
C7 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C7 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C8 C2 H2A 109.5 . .
C8 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C8 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C9 C3 H3A 109.5 . .
C9 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C9 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C10 C4 H4A 109.5 . .
C10 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C10 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 H5A 109.5 . .
C6 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C6 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C10 C6 C7 111.6(8) . .
C10 C6 C5 126.6(11) . .
C7 C6 C5 121.6(11) . .
C10 C6 Fe1 72.7(4) . .
C7 C6 Fe1 70.1(4) . .
C5 C6 Fe1 128.3(6) . .
C6 C7 C1 132.0(14) . .
C6 C7 C8 103.9(6) . .
C1 C7 C8 124.1(13) . .
C6 C7 Fe1 70.7(4) . .
C1 C7 Fe1 122.9(6) . .
C8 C7 Fe1 68.5(4) . .
C9 C8 C2 129.3(11) . .
C9 C8 C7 103.0(6) . .
C2 C8 C7 127.5(11) . .
C9 C8 Fe1 70.7(4) . .
C2 C8 Fe1 127.6(5) . .
C7 C8 Fe1 68.1(4) . .
C10 C9 C8 110.7(7) . .
C10 C9 C3 127.6(8) . .
C8 C9 C3 121.6(8) . .
C10 C9 Fe1 71.9(4) . .
C8 C9 Fe1 70.0(4) . .
C3 C9 Fe1 127.8(5) . .
C6 C10 C9 110.8(7) . .
C6 C10 C4 123.2(10) . .
C9 C10 C4 125.7(10) . .
C6 C10 Fe1 70.9(4) . .
C9 C10 Fe1 70.7(4) . .
C4 C10 Fe1 129.7(6) . .
C12 C11 H11A 108.6 . .
C12 C11 H11B 109.9 . .
H11A C11 H11B 109.5 . .
C11 C12 S2 113.0(7) . .
C11 C12 H12A 109.3 . .
S2 C12 H12A 108.8 . .
C14 C13 H13A 111.0 . .
C14 C13 H13B 108.7 . .
H13A C13 H13B 109.5 . .
C13 C14 S3 115.4(6) . .
C13 C14 H14A 108.1 . .
S3 C14 H14A 108.7 . .
N1 C15 H15A 109.5 . .
N1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
N1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.858(5) .
Fe1 C7 2.069(6) .
Fe1 C8 2.073(6) .
Fe1 C6 2.077(7) .
Fe1 C9 2.083(6) .
Fe1 C10 2.098(7) .
Fe1 S2 2.2841(15) .
Fe1 S3 2.2866(16) .
S2 C12 1.895(9) .
S2 Fe1 2.2841(14) 4_565
S3 C14 1.861(8) .
S3 Fe1 2.2866(16) 4_565
N1 N1 1.308(9) 4_565
N1 C15 1.466(11) .
C1 C7 1.487(12) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C8 1.495(11) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 C9 1.534(11) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 C10 1.512(12) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 C6 1.535(13) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C10 1.304(12) .
C6 C7 1.390(12) .
C7 C8 1.531(13) .
C8 C9 1.398(10) .
C9 C10 1.342(10) .
C11 C12 1.503(14) .
C11 H11A 0.9601 .
C11 H11B 0.9600 .
C12 H12A 0.9600 .
C13 C14 1.495(13) .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C14 H14A 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
