#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/77/4107780.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_4107780
loop_
_publ_author_name
'Ying Yu'
'Azwana R. Sadique'
'Jeremy M. Smith'
'Thomas R. Dugan'
'Ryan E. Cowley'
'William W. Brennessel'
'Christine J. Flaschenriem'
'Eckhard Bill'
'Thomas R. Cundari'
'Patrick L. Holland'
_publ_section_title
;
 The Reactivity Patterns of Low-Coordinate Iron-Hydride Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6624
_journal_page_last               6638
_journal_paper_doi               10.1021/ja710669w
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C59.80 H83.80 Cl0.20 Fe2 N4 O3.60, 2(C7 H8)'
_chemical_formula_sum            'C73.8 H99.8 Cl0.2 Fe2 N4 O3.6'
_chemical_formula_weight         1219.37
_chemical_name_common            holyy23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/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                 124.815(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.222(2)
_cell_length_b                   19.321(2)
_cell_length_c                   13.3145(16)
_cell_measurement_reflns_used    3228
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.84
_cell_measurement_theta_min      2.81
_cell_volume                     3426.1(7)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, ω scans per φ'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22810
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.9101
_exptl_absorpt_correction_T_min  0.8616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             1310
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0546P)²+2.6308P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                4407
_reflns_number_total             5289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja710669w-file004_09.cif
_cod_data_source_block           10a
_cod_original_cell_volume        3426.2(7)
_cod_original_formula_sum        'C73.80 H99.80 Cl0.20 Fe2 N4 O3.60'
_cod_database_code               4107780
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_group
Fe1 Fe 0.06042(3) 0.0000 0.19392(4) 0.02007(10) Uani 0.901(2) 2 d SP 1
C14 C -0.15413(18) 0.0000 -0.04173(19) 0.0282(4) Uani 0.901(2) 2 d SP 1
H1 H -0.2219 0.0000 -0.0667 0.034 Uiso 0.901(2) 2 calc SPR 1
O1 O -0.08894(13) 0.0000 0.07073(13) 0.0300(4) Uani 0.901(2) 2 d SP 1
O2 O -0.14116(14) 0.0000 -0.12535(15) 0.0366(4) Uani 0.901(2) 2 d SP 1
Fe1' Fe 0.0715(4) 0.0000 0.1719(4) 0.02007(10) Uani 0.099(2) 2 d SP 5
Cl1' Cl -0.0738(4) 0.0000 -0.0271(4) 0.0275(14) Uani 0.099(2) 2 d SP 5
N1 N 0.09390(8) 0.07576(5) 0.31097(10) 0.0202(2) Uani 1 1 d . 1
C11 C 0.12276(12) 0.12664(7) 0.49840(13) 0.0288(3) Uani 1 1 d . 1
H11A H 0.1927 0.1418 0.5404 0.043 Uiso 1 1 calc R 1
H11B H 0.1098 0.1129 0.5590 0.043 Uiso 1 1 calc R 1
H11C H 0.0779 0.1648 0.4487 0.043 Uiso 1 1 calc R 1
C21 C 0.10416(9) 0.06568(6) 0.41667(12) 0.0217(2) Uani 1 1 d . 1
C31 C 0.10238(14) 0.0000 0.46095(17) 0.0232(3) Uani 1 2 d S 1
H31 H 0.0996 0.0000 0.5303 0.028 Uiso 1 2 calc SR 1
C12 C 0.10862(9) 0.14397(6) 0.28015(11) 0.0198(2) Uani 1 1 d . 1
C22 C 0.02475(10) 0.18526(6) 0.19833(11) 0.0212(2) Uani 1 1 d . 1
C32 C 0.04075(11) 0.25012(7) 0.16616(12) 0.0256(3) Uani 1 1 d . 1
H32 H -0.0152 0.2784 0.1107 0.031 Uiso 1 1 calc R 1
C42 C 0.13687(11) 0.27396(7) 0.21367(13) 0.0271(3) Uani 1 1 d . 1
H42 H 0.1466 0.3185 0.1918 0.032 Uiso 1 1 calc R 1
C52 C 0.21865(10) 0.23264(7) 0.29321(12) 0.0250(3) Uani 1 1 d . 1
H52 H 0.2844 0.2492 0.3252 0.030 Uiso 1 1 calc R 1
C62 C 0.20659(10) 0.16729(7) 0.32744(12) 0.0222(2) Uani 1 1 d . 1
C72 C -0.08191(10) 0.16198(7) 0.14688(12) 0.0243(3) Uani 1 1 d . 1
H72 H -0.0796 0.1120 0.1678 0.029 Uiso 1 1 calc R 1
C82 C -0.12510(12) 0.20273(9) 0.20565(15) 0.0364(3) Uani 1 1 d . 1
H82A H -0.0820 0.1963 0.2946 0.055 Uiso 1 1 calc R 1
H82B H -0.1929 0.1859 0.1735 0.055 Uiso 1 1 calc R 1
H82C H -0.1280 0.2520 0.1864 0.055 Uiso 1 1 calc R 1
C92 C -0.15063(11) 0.16897(8) 0.00755(13) 0.0323(3) Uani 1 1 d . 1
H92A H -0.1610 0.2181 -0.0148 0.048 Uiso 1 1 calc R 1
H92B H -0.2154 0.1471 -0.0232 0.048 Uiso 1 1 calc R 1
H92C H -0.1194 0.1462 -0.0287 0.048 Uiso 1 1 calc R 1
C102 C 0.29915(10) 0.12319(7) 0.41196(13) 0.0284(3) Uani 1 1 d . 1
H102 H 0.2779 0.0815 0.4362 0.034 Uiso 1 1 calc R 1
C112 C 0.34601(12) 0.09882(9) 0.34584(16) 0.0398(4) Uani 1 1 d . 1
H11D H 0.2956 0.0738 0.2714 0.060 Uiso 1 1 calc R 1
H11E H 0.4028 0.0681 0.3997 0.060 Uiso 1 1 calc R 1
H11F H 0.3697 0.1390 0.3241 0.060 Uiso 1 1 calc R 1
C122 C 0.37841(13) 0.16250(11) 0.52899(15) 0.0426(4) Uani 1 1 d . 1
H12A H 0.4066 0.2001 0.5080 0.064 Uiso 1 1 calc R 1
H12B H 0.4322 0.1306 0.5860 0.064 Uiso 1 1 calc R 1
H12C H 0.3469 0.1818 0.5674 0.064 Uiso 1 1 calc R 1
C15 C 0.2716(4) 0.0000 -0.1785(3) 0.0846(13) Uani 1 2 d S 1
H15A H 0.2586 0.0477 -0.2089 0.127 Uiso 0.50 1 calc PR 1
H15B H 0.2091 -0.0209 -0.1977 0.127 Uiso 0.50 1 calc PR 1
H15C H 0.2972 -0.0268 -0.2177 0.127 Uiso 0.50 1 calc PR 1
C25 C 0.3486(2) 0.0000 -0.0415(3) 0.0523(7) Uani 1 2 d S 1
C35 C 0.3836(2) 0.06126(11) 0.0232(2) 0.0610(6) Uani 1 1 d . 1
H35A H 0.3600 0.1040 -0.0194 0.073 Uiso 1 1 calc R 1
C45 C 0.4520(2) 0.06168(11) 0.1482(2) 0.0707(7) Uani 1 1 d . 1
H45A H 0.4747 0.1044 0.1911 0.085 Uiso 1 1 calc R 1
C55 C 0.4877(3) 0.0000 0.2112(3) 0.0702(10) Uani 1 2 d S 1
H55A H 0.5364 0.0000 0.2972 0.084 Uiso 1 2 calc SR 1
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 N1 95.67(7) 6 .
N1 Fe1 O2 114.07(5) 6 5
N1 Fe1 O2 114.07(5) . 5
N1 Fe1 O1 107.75(5) 6 .
N1 Fe1 O1 107.75(5) . .
O2 Fe1 O1 115.57(7) 5 .
N1 Fe1 Cl1' 127.83(5) 6 5
N1 Fe1 Cl1' 127.83(5) . 5
O2 Fe1 Cl1' 28.59(13) 5 5
O1 Fe1 Cl1' 86.98(13) . 5
O2 C14 O1 127.9(2) . .
O2 C14 H1 116.1 . .
O1 C14 H1 116.1 . .
C14 O1 Fe1 141.53(16) . .
C14 O2 Fe1 155.05(17) . 5
Fe1' Cl1' Fe1 119.6(2) . 5
C21 N1 C12 119.55(10) . .
C21 N1 Fe1 122.47(9) . .
C12 N1 Fe1 117.97(8) . .
N1 C21 C31 123.64(12) . .
N1 C21 C11 119.93(11) . .
C31 C21 C11 116.39(12) . .
C21 C31 C21 128.91(17) . 6
C21 C31 H31 115.5 . .
C21 C31 H31 115.5 6 .
C22 C12 C62 120.68(11) . .
C22 C12 N1 119.65(11) . .
C62 C12 N1 119.59(11) . .
C32 C22 C12 118.64(12) . .
C32 C22 C72 119.38(11) . .
C12 C22 C72 121.97(11) . .
C42 C32 C22 121.11(13) . .
C42 C32 H32 119.4 . .
C22 C32 H32 119.4 . .
C52 C42 C32 119.68(12) . .
C52 C42 H42 120.2 . .
C32 C42 H42 120.2 . .
C42 C52 C62 121.39(12) . .
C42 C52 H52 119.3 . .
C62 C52 H52 119.3 . .
C52 C62 C12 118.49(12) . .
C52 C62 C102 119.05(12) . .
C12 C62 C102 122.45(11) . .
C22 C72 C92 111.97(11) . .
C22 C72 C82 110.63(11) . .
C92 C72 C82 110.16(12) . .
C22 C72 H72 108.0 . .
C92 C72 H72 108.0 . .
C82 C72 H72 108.0 . .
C62 C102 C112 110.57(12) . .
C62 C102 C122 111.93(12) . .
C112 C102 C122 109.39(12) . .
C62 C102 H102 108.3 . .
C112 C102 H102 108.3 . .
C122 C102 H102 108.3 . .
C35 C25 C35 118.0(3) . 6
C35 C25 C15 121.00(14) . .
C35 C25 C15 121.00(14) 6 .
C45 C35 C25 121.4(2) . .
C45 C35 H35A 119.3 . .
C25 C35 H35A 119.3 . .
C35 C45 C55 119.9(2) . .
C35 C45 H45A 120.0 . .
C55 C45 H45A 120.0 . .
C45 C55 C45 119.4(3) . 6
C45 C55 H55A 120.3 . .
C45 C55 H55A 120.3 6 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.9748(11) 6
Fe1 N1 1.9749(11) .
Fe1 O2 1.9785(19) 5
Fe1 O1 2.0057(17) .
Fe1 Cl1' 2.352(4) 5
C14 O2 1.245(3) .
C14 O1 1.246(3) .
C14 H1 0.9500 .
O2 Fe1 1.9785(19) 5
Fe1' Cl1' 2.333(6) .
Cl1' Fe1 2.352(4) 5
N1 C21 1.3338(17) .
N1 C12 1.4402(15) .
C11 C21 1.5125(18) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C21 C31 1.4065(15) .
C31 C21 1.4065(15) 6
C31 H31 0.9500 .
C12 C22 1.4079(17) .
C12 C62 1.4080(17) .
C22 C32 1.3958(18) .
C22 C72 1.5204(18) .
C32 C42 1.385(2) .
C32 H32 0.9500 .
C42 C52 1.384(2) .
C42 H42 0.9500 .
C52 C62 1.3935(18) .
C52 H52 0.9500 .
C62 C102 1.5223(18) .
C72 C92 1.5301(19) .
C72 C82 1.533(2) .
C72 H72 1.0000 .
C82 H82A 0.9800 .
C82 H82B 0.9800 .
C82 H82C 0.9800 .
C92 H92A 0.9800 .
C92 H92B 0.9800 .
C92 H92C 0.9800 .
C102 C112 1.529(2) .
C102 C122 1.540(2) .
C102 H102 1.0000 .
C112 H11D 0.9800 .
C112 H11E 0.9800 .
C112 H11F 0.9800 .
C122 H12A 0.9800 .
C122 H12B 0.9800 .
C122 H12C 0.9800 .
C15 C25 1.512(4) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C25 C35 1.381(3) .
C25 C35 1.381(3) 6
C35 C45 1.376(3) .
C35 H35A 0.9500 .
C45 C55 1.380(3) .
C45 H45A 0.9500 .
C55 C45 1.380(3) 6
C55 H55A 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 C14 O1 Fe1 0.0 . .
N1 Fe1 O1 C14 -128.90(4) 6 .
N1 Fe1 O1 C14 128.90(4) . .
O2 Fe1 O1 C14 0.0 5 .
Cl1' Fe1 O1 C14 0.0 5 .
O1 C14 O2 Fe1 0.0 . 5
N1 Fe1 N1 C21 -16.14(12) 6 .
O2 Fe1 N1 C21 -135.70(10) 5 .
O1 Fe1 N1 C21 94.56(10) . .
Cl1' Fe1 N1 C21 -165.16(16) 5 .
N1 Fe1 N1 C12 163.16(6) 6 .
O2 Fe1 N1 C12 43.59(10) 5 .
O1 Fe1 N1 C12 -86.15(9) . .
Cl1' Fe1 N1 C12 14.14(17) 5 .
C12 N1 C21 C31 -172.64(13) . .
Fe1 N1 C21 C31 6.64(19) . .
C12 N1 C21 C11 4.95(17) . .
Fe1 N1 C21 C11 -175.77(9) . .
N1 C21 C31 C21 9.7(3) . 6
C11 C21 C31 C21 -167.93(15) . 6
C21 N1 C12 C22 -100.55(14) . .
Fe1 N1 C12 C22 80.14(12) . .
C21 N1 C12 C62 82.58(15) . .
Fe1 N1 C12 C62 -96.74(12) . .
C62 C12 C22 C32 -0.72(18) . .
N1 C12 C22 C32 -177.56(11) . .
C62 C12 C22 C72 -179.22(11) . .
N1 C12 C22 C72 3.94(18) . .
C12 C22 C32 C42 -0.30(19) . .
C72 C22 C32 C42 178.24(12) . .
C22 C32 C42 C52 0.8(2) . .
C32 C42 C52 C62 -0.3(2) . .
C42 C52 C62 C12 -0.65(19) . .
C42 C52 C62 C102 178.02(12) . .
C22 C12 C62 C52 1.19(18) . .
N1 C12 C62 C52 178.03(11) . .
C22 C12 C62 C102 -177.44(12) . .
N1 C12 C62 C102 -0.59(18) . .
C32 C22 C72 C92 51.74(16) . .
C12 C22 C72 C92 -129.78(13) . .
C32 C22 C72 C82 -71.56(16) . .
C12 C22 C72 C82 106.93(14) . .
C52 C62 C102 C112 -69.35(16) . .
C12 C62 C102 C112 109.26(15) . .
C52 C62 C102 C122 52.89(17) . .
C12 C62 C102 C122 -128.50(14) . .
C35 C25 C35 C45 0.6(5) 6 .
C15 C25 C35 C45 178.6(3) . .
C25 C35 C45 C55 0.6(5) . .
C35 C45 C55 C45 -1.8(6) . 6
