#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:52:13 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179428 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/25/4332554.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332554
loop_
_publ_author_name
'Hung, Mu-Cheng'
'Tsai, Ming-Che'
'Lee, Gene-Hsiang'
'Liaw, Wen-Feng'
_publ_section_title
;
 Transformation and Structural Discrimination between the Neutral
 {Fe(NO)2}10Dinitrosyliron Complexes (DNICs) and the Anionic/Cationic
 {Fe(NO)2}9DNICs
;
_journal_issue                   15
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6041
_journal_page_last               6047
_journal_paper_doi               10.1021/ic0605120
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C15 H26 Fe N4 O2'
_chemical_formula_weight         350.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0599(6)
_cell_length_b                   13.3528(9)
_cell_length_c                   14.5948(10)
_cell_measurement_reflns_used    4442
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.79
_cell_volume                     1570.72(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      150(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       '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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15745
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.8291
_exptl_absorpt_correction_T_min  0.7589
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3621
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0332
_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)+(0.0424P)²+0.0817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0792
_reflns_number_gt                3468
_reflns_number_total             3621
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0605120sup1.cif
_cod_data_source_block           ic11472
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1570.73(19)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4332554
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'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
Fe Fe 0.96215(4) 0.12388(2) 0.30371(2) 0.01701(9) Uani 1 1 d .
N1 N 1.0868(2) 0.21529(14) 0.33607(13) 0.0222(4) Uani 1 1 d .
N2 N 1.0173(2) 0.07585(14) 0.20464(13) 0.0243(4) Uani 1 1 d .
N3 N 0.9026(2) 0.01661(12) 0.40683(12) 0.0150(3) Uani 1 1 d .
N4 N 0.7001(2) 0.14395(12) 0.29654(12) 0.0172(3) Uani 1 1 d .
O1 O 1.2051(7) 0.2705(4) 0.3379(4) 0.0274(14) Uiso 0.50 1 d P
O2 O 1.0567(6) 0.0461(3) 0.1291(3) 0.0323(11) Uiso 0.50 1 d P
O1' O 1.1808(7) 0.2866(4) 0.3415(4) 0.0302(15) Uiso 0.50 1 d P
O2' O 1.0943(6) 0.0651(3) 0.1336(3) 0.0335(12) Uiso 0.50 1 d P
C1 C 1.0680(3) -0.01789(15) 0.43979(15) 0.0195(4) Uani 1 1 d .
H1A H 1.1214 0.0378 0.4735 0.023 Uiso 1 1 calc R
H1B H 1.1381 -0.0331 0.3858 0.023 Uiso 1 1 calc R
C2 C 1.0648(3) -0.10990(16) 0.50192(16) 0.0250(5) Uani 1 1 d .
H2A H 1.1797 -0.1292 0.5183 0.030 Uiso 1 1 calc R
H2B H 1.0044 -0.0941 0.5592 0.030 Uiso 1 1 calc R
C3 C 0.9797(3) -0.19628(16) 0.45285(17) 0.0258(5) Uani 1 1 d .
H3A H 0.9699 -0.2542 0.4949 0.031 Uiso 1 1 calc R
H3B H 1.0470 -0.2171 0.3994 0.031 Uiso 1 1 calc R
C4 C 0.8079(3) -0.16422(16) 0.42093(16) 0.0242(5) Uani 1 1 d .
H4A H 0.7369 -0.1521 0.4751 0.029 Uiso 1 1 calc R
H4B H 0.7573 -0.2193 0.3850 0.029 Uiso 1 1 calc R
C5 C 0.8126(3) -0.06910(15) 0.36188(15) 0.0183(4) Uani 1 1 d .
H5A H 0.8738 -0.0859 0.3043 0.022 Uiso 1 1 calc R
C6 C 0.6376(3) -0.03668(16) 0.33449(15) 0.0205(5) Uani 1 1 d .
H6A H 0.5798 -0.0964 0.3082 0.025 Uiso 1 1 calc R
C7 C 0.5394(3) -0.00255(15) 0.41837(15) 0.0225(4) Uani 1 1 d .
H7A H 0.4241 0.0146 0.4010 0.027 Uiso 1 1 calc R
H7B H 0.5363 -0.0562 0.4651 0.027 Uiso 1 1 calc R
C8 C 0.6290(3) 0.08941(15) 0.45550(14) 0.0178(4) Uani 1 1 d .
H8A H 0.5691 0.1120 0.5118 0.021 Uiso 1 1 calc R
C9 C 0.6176(3) 0.17344(15) 0.38467(14) 0.0185(4) Uani 1 1 d .
H9A H 0.4972 0.1834 0.3709 0.022 Uiso 1 1 calc R
C10 C 0.6843(3) 0.27320(15) 0.41786(15) 0.0214(5) Uani 1 1 d .
H10A H 0.8052 0.2675 0.4289 0.026 Uiso 1 1 calc R
H10B H 0.6304 0.2912 0.4765 0.026 Uiso 1 1 calc R
C11 C 0.6517(3) 0.35546(16) 0.34724(16) 0.0252(5) Uani 1 1 d .
H11A H 0.5308 0.3669 0.3413 0.030 Uiso 1 1 calc R
H11B H 0.7039 0.4188 0.3675 0.030 Uiso 1 1 calc R
C12 C 0.7231(3) 0.32410(17) 0.25542(15) 0.0242(5) Uani 1 1 d .
H12A H 0.6909 0.3737 0.2083 0.029 Uiso 1 1 calc R
H12B H 0.8458 0.3235 0.2594 0.029 Uiso 1 1 calc R
C13 C 0.6630(3) 0.22154(17) 0.22668(15) 0.0233(5) Uani 1 1 d .
H13A H 0.5417 0.2241 0.2162 0.028 Uiso 1 1 calc R
H13B H 0.7167 0.2028 0.1681 0.028 Uiso 1 1 calc R
C14 C 0.8049(3) 0.06031(15) 0.48350(14) 0.0174(4) Uani 1 1 d .
H14A H 0.8631 0.1205 0.5067 0.021 Uiso 1 1 calc R
H14B H 0.7991 0.0111 0.5341 0.021 Uiso 1 1 calc R
C15 C 0.6310(3) 0.04684(16) 0.26300(15) 0.0214(4) Uani 1 1 d .
H15A H 0.6940 0.0255 0.2082 0.026 Uiso 1 1 calc R
H15B H 0.5142 0.0572 0.2442 0.026 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'
O O 0.0106 0.0060 '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
N2 Fe N1 112.08(10)
N2 Fe N4 105.90(8)
N1 Fe N4 121.63(8)
N2 Fe N3 114.82(8)
N1 Fe N3 115.59(8)
N4 Fe N3 84.03(7)
O1 N1 O1' 14.0(4)
O1 N1 Fe 160.1(3)
O1' N1 Fe 167.1(3)
O2 N2 O2' 18.9(3)
O2 N2 Fe 176.0(3)
O2' N2 Fe 159.0(3)
C14 N3 C1 110.60(16)
C14 N3 C5 111.77(16)
C1 N3 C5 109.68(16)
C14 N3 Fe 112.74(12)
C1 N3 Fe 103.53(12)
C5 N3 Fe 108.16(12)
C13 N4 C15 107.81(16)
C13 N4 C9 108.46(16)
C15 N4 C9 110.10(16)
C13 N4 Fe 108.72(13)
C15 N4 Fe 106.03(12)
C9 N4 Fe 115.45(13)
N3 C1 C2 115.18(17)
C3 C2 C1 109.76(19)
C2 C3 C4 109.95(18)
C3 C4 C5 112.46(19)
N3 C5 C6 110.08(16)
N3 C5 C4 113.34(18)
C6 C5 C4 111.00(18)
C7 C6 C15 108.14(18)
C7 C6 C5 110.67(18)
C15 C6 C5 114.67(18)
C8 C7 C6 106.25(18)
C7 C8 C14 109.30(17)
C7 C8 C9 108.81(17)
C14 C8 C9 115.09(18)
N4 C9 C10 110.33(17)
N4 C9 C8 111.14(16)
C10 C9 C8 114.05(18)
C9 C10 C11 110.78(18)
C12 C11 C10 109.36(17)
C13 C12 C11 111.92(19)
N4 C13 C12 112.15(18)
N3 C14 C8 112.97(17)
N4 C15 C6 113.38(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe N2 1.6430(19)
Fe N1 1.6501(19)
Fe N4 2.1319(18)
Fe N3 2.1324(17)
N1 O1 1.206(6)
N1 O1' 1.220(6)
N2 O2 1.214(5)
N2 O2' 1.217(5)
N3 C14 1.487(3)
N3 C1 1.490(3)
N3 C5 1.505(2)
N4 C13 1.484(3)
N4 C15 1.494(3)
N4 C9 1.500(3)
C1 C2 1.527(3)
C2 C3 1.521(3)
C3 C4 1.523(3)
C4 C5 1.535(3)
C5 C6 1.528(3)
C6 C7 1.527(3)
C6 C15 1.528(3)
C7 C8 1.524(3)
C8 C14 1.525(3)
C8 C9 1.528(3)
C9 C10 1.516(3)
C10 C11 1.529(3)
C11 C12 1.518(3)
C12 C13 1.512(3)
