#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:47:27 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178916 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/45/4114533.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_4114533
loop_
_publ_author_name
'Jeremy M. Smith'
'Rene J. Lachicotte'
'Patrick L. Holland'
_publ_section_title
;
 NN Bond Cleavage by a Low-Coordinate Iron(II) Hydride Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15752
_journal_page_last               15753
_journal_paper_doi               10.1021/ja038152s
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C35 H54 Fe N2'
_chemical_formula_weight         558.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.584(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.130(2)
_cell_length_b                   12.2104(11)
_cell_length_c                   26.171(3)
_cell_measurement_temperature    193(2)
_cell_volume                     7170.2(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15766
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   'empirical; SADABS'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.570
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.426
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.426
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.1219
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0309P)²+63.5901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2251
_reflns_number_gt                4622
_reflns_number_total             5131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038152ssi20030827_085523_1.cif
_cod_data_source_block           '[LFeH]2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'na' 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_database_code               4114533
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.05536(4) 0.94568(8) 0.28490(4) 0.0296(3) Uani 1 1 d .
H1 H 0.015(3) 0.938(6) 0.236(3) 0.07(3) Uiso 1 1 d .
N1 N 0.1277(2) 0.8664(4) 0.2820(2) 0.0315(14) Uani 1 1 d .
N2 N 0.1007(2) 1.0408(5) 0.3482(2) 0.0348(14) Uani 1 1 d .
C11 C 0.2428(3) 0.8531(7) 0.3098(4) 0.058(2) Uani 1 1 d .
C21 C 0.1820(3) 0.9080(6) 0.3054(3) 0.0393(19) Uani 1 1 d .
C31 C 0.1902(3) 1.0110(6) 0.3326(3) 0.043(2) Uani 1 1 d .
H31A H 0.2260 1.0444 0.3358 0.051 Uiso 1 1 calc R
C41 C 0.1571(3) 1.0729(6) 0.3553(3) 0.0391(18) Uani 1 1 d .
C51 C 0.1899(3) 1.1775(7) 0.3856(3) 0.047(2) Uani 1 1 d .
C61 C 0.2741(5) 0.9273(9) 0.2814(6) 0.121(6) Uani 1 1 d .
H61A H 0.3078 0.8894 0.2786 0.182 Uiso 1 1 calc R
H61B H 0.2874 0.9929 0.3026 0.182 Uiso 1 1 calc R
H61C H 0.2468 0.9459 0.2453 0.182 Uiso 1 1 calc R
C71 C 0.2802(4) 0.8405(11) 0.3710(5) 0.115(5) Uani 1 1 d .
H71A H 0.3174 0.8063 0.3754 0.173 Uiso 1 1 calc R
H71B H 0.2590 0.7959 0.3880 0.173 Uiso 1 1 calc R
H71C H 0.2874 0.9114 0.3881 0.173 Uiso 1 1 calc R
C81 C 0.2415(4) 0.7394(7) 0.2846(4) 0.063(3) Uani 1 1 d .
H81A H 0.2814 0.7163 0.2908 0.095 Uiso 1 1 calc R
H81B H 0.2189 0.7424 0.2458 0.095 Uiso 1 1 calc R
H81C H 0.2233 0.6882 0.3015 0.095 Uiso 1 1 calc R
C91 C 0.2573(4) 1.1597(8) 0.4169(4) 0.075(3) Uani 1 1 d .
H91A H 0.2767 1.1508 0.3910 0.112 Uiso 1 1 calc R
H91B H 0.2634 1.0952 0.4392 0.112 Uiso 1 1 calc R
H91C H 0.2738 1.2220 0.4398 0.112 Uiso 1 1 calc R
C101 C 0.1831(4) 1.2610(7) 0.3396(4) 0.059(2) Uani 1 1 d .
H10A H 0.1986 1.2303 0.3138 0.088 Uiso 1 1 calc R
H10B H 0.2046 1.3265 0.3552 0.088 Uiso 1 1 calc R
H10C H 0.1416 1.2782 0.3210 0.088 Uiso 1 1 calc R
C111 C 0.1666(4) 1.2332(8) 0.4265(4) 0.070(3) Uani 1 1 d .
H11A H 0.1250 1.2498 0.4084 0.105 Uiso 1 1 calc R
H11B H 0.1883 1.2997 0.4398 0.105 Uiso 1 1 calc R
H11C H 0.1718 1.1848 0.4569 0.105 Uiso 1 1 calc R
C12 C 0.1159(3) 0.7643(6) 0.2519(3) 0.042(2) Uani 1 1 d .
C22 C 0.1100(3) 0.6672(6) 0.2779(4) 0.047(2) Uani 1 1 d .
C32 C 0.0992(4) 0.5709(7) 0.2471(5) 0.074(3) Uani 1 1 d .
H32A H 0.0960 0.5052 0.2638 0.089 Uiso 1 1 calc R
C42 C 0.0932(4) 0.5704(10) 0.1931(6) 0.084(4) Uani 1 1 d .
H42A H 0.0866 0.5048 0.1737 0.101 Uiso 1 1 calc R
C52 C 0.0969(4) 0.6655(9) 0.1681(4) 0.068(3) Uani 1 1 d .
H52A H 0.0920 0.6640 0.1311 0.082 Uiso 1 1 calc R
C62 C 0.1078(3) 0.7651(7) 0.1954(4) 0.051(2) Uani 1 1 d .
C72 C 0.1143(3) 0.6661(7) 0.3373(4) 0.060(3) Uani 1 1 d .
H72A H 0.1288 0.7379 0.3534 0.072 Uiso 1 1 calc R
C82 C 0.0521(4) 0.6486(9) 0.3394(5) 0.082(3) Uani 1 1 d .
H82A H 0.0246 0.6999 0.3154 0.123 Uiso 1 1 calc R
H82B H 0.0539 0.6595 0.3763 0.123 Uiso 1 1 calc R
H82C H 0.0389 0.5753 0.3278 0.123 Uiso 1 1 calc R
C92 C 0.1574(5) 0.5794(9) 0.3719(5) 0.099(4) Uani 1 1 d .
H92A H 0.1962 0.5917 0.3707 0.148 Uiso 1 1 calc R
H92B H 0.1435 0.5080 0.3574 0.148 Uiso 1 1 calc R
H92C H 0.1596 0.5839 0.4092 0.148 Uiso 1 1 calc R
C102 C 0.1088(4) 0.8694(9) 0.1649(4) 0.063(3) Uani 1 1 d .
H10D H 0.1183 0.9301 0.1912 0.076 Uiso 1 1 calc R
C112 C 0.1558(5) 0.8679(12) 0.1371(5) 0.117(5) Uani 1 1 d .
H11D H 0.1951 0.8644 0.1648 0.175 Uiso 1 1 calc R
H11E H 0.1521 0.9333 0.1157 0.175 Uiso 1 1 calc R
H11F H 0.1493 0.8051 0.1135 0.175 Uiso 1 1 calc R
C122 C 0.0475(5) 0.8913(10) 0.1206(4) 0.092(4) Uani 1 1 d .
H12A H 0.0184 0.8978 0.1374 0.138 Uiso 1 1 calc R
H12B H 0.0368 0.8317 0.0949 0.138 Uiso 1 1 calc R
H12C H 0.0488 0.9580 0.1017 0.138 Uiso 1 1 calc R
C13 C 0.0754(3) 1.0718(6) 0.3887(3) 0.0355(18) Uani 1 1 d .
C23 C 0.0289(4) 1.1448(6) 0.3779(3) 0.0422(19) Uani 1 1 d .
C33 C 0.0072(4) 1.1692(8) 0.4192(3) 0.062(3) Uani 1 1 d .
H33A H -0.0236 1.2197 0.4122 0.075 Uiso 1 1 calc R
C43 C 0.0304(5) 1.1202(9) 0.4700(4) 0.072(3) Uani 1 1 d .
H43A H 0.0163 1.1397 0.4974 0.086 Uiso 1 1 calc R
C53 C 0.0735(4) 1.0439(10) 0.4802(3) 0.070(3) Uani 1 1 d .
H53A H 0.0875 1.0088 0.5141 0.084 Uiso 1 1 calc R
C63 C 0.0978(4) 1.0161(6) 0.4403(3) 0.043(2) Uani 1 1 d .
C73 C 0.0011(4) 1.2032(8) 0.3230(3) 0.055(2) Uani 1 1 d .
H73A H 0.0201 1.1755 0.2983 0.066 Uiso 1 1 calc R
C83 C -0.0651(4) 1.1797(11) 0.2970(4) 0.089(4) Uani 1 1 d .
H83A H -0.0719 1.1027 0.2991 0.134 Uiso 1 1 calc R
H83B H -0.0796 1.2019 0.2591 0.134 Uiso 1 1 calc R
H83C H -0.0858 1.2196 0.3161 0.134 Uiso 1 1 calc R
C93 C 0.0118(6) 1.3277(9) 0.3293(5) 0.100(4) Uani 1 1 d .
H93A H 0.0537 1.3418 0.3468 0.150 Uiso 1 1 calc R
H93B H -0.0088 1.3574 0.3514 0.150 Uiso 1 1 calc R
H93C H -0.0030 1.3616 0.2937 0.150 Uiso 1 1 calc R
C103 C 0.1436(4) 0.9232(8) 0.4527(4) 0.066(3) Uani 1 1 d .
H10E H 0.1542 0.9131 0.4202 0.079 Uiso 1 1 calc R
C113 C 0.2013(5) 0.9498(11) 0.5021(5) 0.124(5) Uani 1 1 d .
H11G H 0.2273 0.8874 0.5103 0.187 Uiso 1 1 calc R
H11H H 0.1915 0.9675 0.5335 0.187 Uiso 1 1 calc R
H11I H 0.2210 1.0111 0.4931 0.187 Uiso 1 1 calc R
C123 C 0.1190(5) 0.8151(9) 0.4643(5) 0.106(4) Uani 1 1 d .
H12D H 0.0894 0.7879 0.4310 0.159 Uiso 1 1 calc R
H12E H 0.1014 0.8264 0.4913 0.159 Uiso 1 1 calc R
H12F H 0.1508 0.7628 0.4779 0.159 Uiso 1 1 calc R
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'
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_3
N2 Fe1 N1 95.3(2) .
N2 Fe1 Fe1 133.41(17) 2
N1 Fe1 Fe1 130.22(16) 2
C21 N1 C12 123.0(6) .
C21 N1 Fe1 121.3(5) .
C12 N1 Fe1 115.7(4) .
C41 N2 C13 119.5(6) .
C41 N2 Fe1 119.8(5) .
C13 N2 Fe1 120.6(4) .
C81 C11 C71 105.7(8) .
C81 C11 C61 105.2(8) .
C71 C11 C61 111.1(9) .
C81 C11 C21 118.9(7) .
C71 C11 C21 107.0(7) .
C61 C11 C21 108.9(8) .
N1 C21 C31 120.0(7) .
N1 C21 C11 127.2(7) .
C31 C21 C11 112.7(7) .
C41 C31 C21 134.7(7) .
N2 C41 C31 119.4(7) .
N2 C41 C51 126.9(7) .
C31 C41 C51 113.6(6) .
C101 C51 C111 106.9(7) .
C101 C51 C91 107.3(7) .
C111 C51 C91 106.1(7) .
C101 C51 C41 104.8(6) .
C111 C51 C41 117.9(6) .
C91 C51 C41 113.2(7) .
C22 C12 C62 120.8(7) .
C22 C12 N1 120.1(7) .
C62 C12 N1 119.1(7) .
C32 C22 C12 117.7(9) .
C32 C22 C72 120.7(9) .
C12 C22 C72 121.6(7) .
C42 C32 C22 121.8(10) .
C52 C42 C32 119.8(10) .
C42 C52 C62 122.5(10) .
C52 C62 C12 117.3(9) .
C52 C62 C102 120.3(9) .
C12 C62 C102 122.3(7) .
C22 C72 C92 112.8(9) .
C22 C72 C82 109.8(7) .
C92 C72 C82 110.2(8) .
C62 C102 C122 110.5(9) .
C62 C102 C112 113.1(8) .
C122 C102 C112 108.4(8) .
C23 C13 C63 119.9(7) .
C23 C13 N2 123.1(6) .
C63 C13 N2 116.8(7) .
C13 C23 C33 119.2(7) .
C13 C23 C73 122.8(6) .
C33 C23 C73 118.0(7) .
C43 C33 C23 121.3(9) .
C53 C43 C33 120.2(9) .
C43 C53 C63 121.3(9) .
C53 C63 C13 117.9(8) .
C53 C63 C103 119.0(8) .
C13 C63 C103 123.0(7) .
C83 C73 C23 111.3(8) .
C83 C73 C93 110.0(9) .
C23 C73 C93 111.3(8) .
C123 C103 C63 112.3(8) .
C123 C103 C113 108.2(8) .
C63 C103 C113 112.2(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.990(5) .
Fe1 N1 2.022(6) .
Fe1 Fe1 2.6236(19) 2
N1 C21 1.328(9) .
N1 C12 1.445(9) .
N2 C41 1.361(9) .
N2 C13 1.456(9) .
C11 C81 1.532(12) .
C11 C71 1.531(14) .
C11 C61 1.535(14) .
C11 C21 1.577(11) .
C21 C31 1.422(10) .
C31 C41 1.383(10) .
C41 C51 1.558(10) .
C51 C101 1.539(11) .
C51 C111 1.541(11) .
C51 C91 1.544(12) .
C12 C22 1.400(11) .
C12 C62 1.420(11) .
C22 C32 1.395(12) .
C22 C72 1.521(12) .
C32 C42 1.366(15) .
C42 C52 1.354(15) .
C52 C62 1.385(12) .
C62 C102 1.508(13) .
C72 C92 1.526(12) .
C72 C82 1.536(12) .
C102 C122 1.530(12) .
C102 C112 1.558(12) .
C13 C23 1.378(10) .
C13 C63 1.428(10) .
C23 C33 1.396(10) .
C23 C73 1.520(11) .
C33 C43 1.375(12) .
C43 C53 1.347(13) .
C53 C63 1.413(12) .
C63 C103 1.534(12) .
C73 C83 1.515(13) .
C73 C93 1.542(14) .
C103 C123 1.523(14) .
C103 C113 1.546(14) .
