#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:16:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179320 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/17/4321731.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_4321731
loop_
_publ_author_name
'Mary K. Ellison'
'Charles E. Schulz'
'W. Robert Scheidt'
_publ_section_title
;
 Syntheses, Characterization, and Structural Studies of Several
 (Nitro)(nitrosyl)iron(III) Porphyrinates: [Fe(Porph)(NO2)(NO)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              100
_journal_page_last               108
_journal_paper_doi               10.1021/ic981162n
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C49 H38 Cl2 Fe N6 O7'
_chemical_formula_weight         949.60
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.620(3)
_cell_length_b                   15.620(3)
_cell_length_c                   18.649(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      -20.5
_cell_volume                     4550.1(13)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        'MADNES (Messerschmitt & Pflugrath, 1987)'
_computing_molecular_graphics    'ORTEP-III (Burnett, Johnson, 1996)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Enraf-Nonius FAST area-detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16096
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        'no measurable crystal decay'
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'square pyramid'
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.116
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3064
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_obs          0.0592
_refine_ls_shift/esd_max         -1.600
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0836P)²+9.1956P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1818
_refine_ls_wR_factor_obs         0.1539
_reflns_number_observed          2279
_reflns_number_total             3068
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981162n_1.cif
_cod_data_source_block           sd:tmeoppnono2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+9.1956P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+9.1956P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4549.8(14)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4321731
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe Fe 0.5000 0.7500 0.1250 0.0239(2) Uani 1 d S .
N(1) N 0.54359(12) 0.62978(12) 0.12386(10) 0.0178(4) Uani 1 d . .
N(2) N 0.5000 0.7500 0.0260(2) 0.0341(7) Uani 1 d S .
O(1) O 0.4663(3) 0.6899(3) -0.0102(2) 0.0322(8) Uani 0.50 d P .
O(2) O 0.5132(8) 0.7710(7) -0.0317(6) 0.057(3) Uiso 0.25 d P .
C(m1) C 0.40667(14) 0.55061(14) 0.12270(11) 0.0191(4) Uani 1 d . .
C(a1) C 0.49555(15) 0.55571(14) 0.12356(11) 0.0197(4) Uani 1 d . .
C(a2) C 0.62751(14) 0.60366(14) 0.12700(11) 0.0192(4) Uani 1 d . .
C(b1) C 0.5511(2) 0.48238(15) 0.12657(13) 0.0235(5) Uani 1 d . .
H(b1) H 0.5339(2) 0.42402(15) 0.12655(13) 0.028 Uiso 1 calc R .
C(b2) C 0.6317(2) 0.51195(15) 0.12941(13) 0.0240(5) Uani 1 d . .
H(b2) H 0.6822(2) 0.47832(15) 0.13246(13) 0.029 Uiso 1 calc R .
C(11) C 0.36548(14) 0.46412(14) 0.12439(12) 0.0201(4) Uani 1 d . .
C(12) C 0.3684(2) 0.4108(2) 0.06504(13) 0.0251(5) Uani 1 d . .
H(12) H 0.3976(2) 0.4290(2) 0.02302(13) 0.030 Uiso 1 calc R .
C(13) C 0.3289(2) 0.3309(2) 0.06643(13) 0.0272(5) Uani 1 d . .
H(13) H 0.3307(2) 0.2952(2) 0.02523(13) 0.033 Uiso 1 calc R .
C(14) C 0.2873(2) 0.30351(15) 0.12731(13) 0.0251(5) Uani 1 d . .
C(15) C 0.2846(2) 0.3557(2) 0.18733(14) 0.0279(5) Uani 1 d . .
H(15) H 0.2567(2) 0.3366(2) 0.22968(14) 0.034 Uiso 1 calc R .
C(16) C 0.3227(2) 0.4359(2) 0.18555(13) 0.0257(5) Uani 1 d . .
H(16) H 0.3196(2) 0.4720(2) 0.22647(13) 0.031 Uiso 1 calc R .
C(17) C 0.2410(2) 0.1751(2) 0.0707(2) 0.0433(7) Uani 1 d . .
H(17)A H 0.2088(14) 0.1228(8) 0.0813(4) 0.065 Uiso 1 calc R .
H(17)B H 0.2983(2) 0.1599(14) 0.0535(8) 0.065 Uiso 1 calc R .
H(17)C H 0.2110(15) 0.2080(6) 0.0336(5) 0.065 Uiso 1 calc R .
O(3) O 0.24821(14) 0.22549(12) 0.13402(10) 0.0361(5) Uani 1 d . .
Cl(1) Cl 0.0000 0.7500 0.0459(3) 0.114(2) Uani 0.40 d SP .
Cl(2) Cl 0.0000 0.7500 -0.0883(4) 0.203(4) Uani 0.50 d SP .
C(18) C -0.0122(8) 0.7200(9) -0.0299(7) 0.022(2) Uiso 0.20 d P .
H(18)A H 0.0198(8) 0.6654(9) -0.0313(7) 0.027 Uiso 0.20 calc PR .
H(18)B H -0.0734(8) 0.7035(9) -0.0313(7) 0.027 Uiso 0.20 calc PR .
Cl(3) Cl 0.0319(9) 0.7408(9) -0.0197(7) 0.031(3) Uiso 0.05 d P .
C(19) C 0.0367(40) 0.6702(41) -0.0719(34) 0.038(12) Uiso 0.05 d P .
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'
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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
N(2) Fe N(2) 180.0 15_565 . ?
N(2) Fe N(1) 89.39(5) 15_565 15_565 ?
N(2) Fe N(1) 90.60(5) . 15_565 ?
N(2) Fe N(1) 90.61(5) 15_565 . ?
N(2) Fe N(1) 89.39(5) . . ?
N(1) Fe N(1) 90.0 15_565 . ?
N(2) Fe N(1) 89.40(5) 15_565 12_766 ?
N(2) Fe N(1) 90.60(5) . 12_766 ?
N(1) Fe N(1) 178.79(10) 15_565 12_766 ?
N(1) Fe N(1) 90.006(1) . 12_766 ?
N(2) Fe N(1) 90.61(5) 15_565 6_564 ?
N(2) Fe N(1) 89.39(5) . 6_564 ?
N(1) Fe N(1) 90.0 15_565 6_564 ?
N(1) Fe N(1) 178.78(10) . 6_564 ?
N(1) Fe N(1) 90.006(1) 12_766 6_564 ?
C(a2) N(1) C(a1) 105.7(2) . . ?
C(a2) N(1) Fe 127.14(15) . . ?
C(a1) N(1) Fe 127.11(15) . . ?
O(2) N(2) O(2) 39.5(11) . 6_564 ?
O(2) N(2) O(1) 77.7(7) . . ?
O(2) N(2) O(1) 38.2(5) 6_564 . ?
O(2) N(2) O(1) 38.2(5) . 6_564 ?
O(2) N(2) O(1) 77.7(7) 6_564 6_564 ?
O(1) N(2) O(1) 115.9(5) . 6_564 ?
O(2) N(2) Fe 160.2(6) . . ?
O(2) N(2) Fe 160.2(6) 6_564 . ?
O(1) N(2) Fe 122.1(2) . . ?
O(1) N(2) Fe 122.1(2) 6_564 . ?
O(2) O(1) N(2) 62.3(8) 6_564 . ?
O(2) O(1) O(2) 15.0(6) 6_564 . ?
N(2) O(1) O(2) 47.5(5) . . ?
O(2) O(2) O(1) 149.5(9) 6_564 6_564 ?
O(2) O(2) N(2) 70.3(6) 6_564 . ?
O(1) O(2) N(2) 79.5(10) 6_564 . ?
O(2) O(2) O(1) 15.5(5) 6_564 . ?
O(1) O(2) O(1) 134.3(12) 6_564 . ?
N(2) O(2) O(1) 54.9(5) . . ?
C(a1) C(m1) C(a2) 123.1(2) . 15_565 ?
C(a1) C(m1) C(11) 118.7(2) . . ?
C(a2) C(m1) C(11) 118.1(2) 15_565 . ?
N(1) C(a1) C(m1) 126.2(2) . . ?
N(1) C(a1) C(b1) 109.9(2) . . ?
C(m1) C(a1) C(b1) 123.8(2) . . ?
N(1) C(a2) C(m1) 126.3(2) . 12_766 ?
N(1) C(a2) C(b2) 109.9(2) . . ?
C(m1) C(a2) C(b2) 123.8(2) 12_766 . ?
C(b2) C(b1) C(a1) 107.0(2) . . ?
C(b1) C(b2) C(a2) 107.5(2) . . ?
C(12) C(11) C(16) 118.7(2) . . ?
C(12) C(11) C(m1) 120.8(2) . . ?
C(16) C(11) C(m1) 120.6(2) . . ?
C(11) C(12) C(13) 120.6(2) . . ?
C(14) C(13) C(12) 120.2(2) . . ?
O(3) C(14) C(13) 124.2(2) . . ?
O(3) C(14) C(15) 115.9(2) . . ?
C(13) C(14) C(15) 119.8(2) . . ?
C(14) C(15) C(16) 120.0(2) . . ?
C(15) C(16) C(11) 120.7(2) . . ?
C(14) O(3) C(17) 116.8(2) . . ?
Cl(3) Cl(1) Cl(3) 45.9(13) 6_464 . ?
Cl(3) Cl(1) C(18) 28.2(6) 6_464 . ?
Cl(3) Cl(1) C(18) 31.5(6) . . ?
Cl(3) Cl(1) C(18) 31.5(6) 6_464 6_464 ?
Cl(3) Cl(1) C(18) 28.2(6) . 6_464 ?
C(18) Cl(1) C(18) 39.4(10) . 6_464 ?
C(18) Cl(2) C(18) 49.8(13) 6_464 . ?
C(18) Cl(2) Cl(2) 155.1(7) 6_464 11_565 ?
C(18) Cl(2) Cl(2) 155.1(7) . 11_565 ?
C(18) Cl(2) Cl(3) 30.9(7) 6_464 . ?
C(18) Cl(2) Cl(3) 34.5(7) . . ?
Cl(2) Cl(2) Cl(3) 158.0(6) 11_565 . ?
C(18) Cl(2) Cl(3) 34.5(7) 6_464 6_464 ?
C(18) Cl(2) Cl(3) 30.9(7) . 6_464 ?
Cl(2) Cl(2) Cl(3) 158.0(6) 11_565 6_464 ?
Cl(3) Cl(2) Cl(3) 44.1(12) . 6_464 ?
C(18) Cl(2) C(19) 61.5(26) 6_464 6_464 ?
C(18) Cl(2) C(19) 94.8(27) . 6_464 ?
Cl(2) Cl(2) C(19) 102.5(26) 11_565 6_464 ?
Cl(3) Cl(2) C(19) 92.1(26) . 6_464 ?
Cl(3) Cl(2) C(19) 63.9(26) 6_464 6_464 ?
C(18) Cl(2) C(19) 94.8(27) 6_464 . ?
C(18) Cl(2) C(19) 61.5(26) . . ?
Cl(2) Cl(2) C(19) 102.6(26) 11_565 . ?
Cl(3) Cl(2) C(19) 63.9(26) . . ?
Cl(3) Cl(2) C(19) 92.1(26) 6_464 . ?
C(19) Cl(2) C(19) 154.9(51) 6_464 . ?
C(18) Cl(2) C(19) 120.4(18) 6_464 16_665 ?
C(18) Cl(2) C(19) 153.7(18) . 16_665 ?
Cl(2) Cl(2) C(19) 39.3(17) 11_565 16_665 ?
Cl(3) Cl(2) C(19) 122.4(18) . 16_665 ?
Cl(3) Cl(2) C(19) 153.8(18) 6_464 16_665 ?
C(19) Cl(2) C(19) 99.7(21) 6_464 16_665 ?
C(19) Cl(2) C(19) 99.7(22) . 16_665 ?
C(18) Cl(2) C(19) 153.7(18) 6_464 11_565 ?
C(18) Cl(2) C(19) 120.4(18) . 11_565 ?
Cl(2) Cl(2) C(19) 39.3(17) 11_565 11_565 ?
Cl(3) Cl(2) C(19) 153.8(18) . 11_565 ?
Cl(3) Cl(2) C(19) 122.4(18) 6_464 11_565 ?
C(19) Cl(2) C(19) 99.7(22) 6_464 11_565 ?
C(19) Cl(2) C(19) 99.7(22) . 11_565 ?
C(19) Cl(2) C(19) 78.7(34) 16_665 11_565 ?
Cl(2) C(18) Cl(1) 135.4(11) . . ?
C(18) Cl(3) Cl(3) 49.2(16) 6_464 6_464 ?
C(18) Cl(3) Cl(1) 89.5(17) 6_464 . ?
Cl(3) Cl(3) Cl(1) 67.1(7) 6_464 . ?
C(18) Cl(3) Cl(2) 60.5(15) 6_464 . ?
Cl(3) Cl(3) Cl(2) 68.0(6) 6_464 . ?
Cl(1) Cl(3) Cl(2) 135.0(12) . . ?
C(18) Cl(3) C(19) 119.4(31) 6_464 . ?
Cl(3) Cl(3) C(19) 104.8(28) 6_464 . ?
Cl(1) Cl(3) C(19) 135.1(26) . . ?
Cl(2) Cl(3) C(19) 58.9(26) . . ?
C(18) Cl(3) C(19) 16.9(23) 6_464 6_464 ?
Cl(3) Cl(3) C(19) 45.2(20) 6_464 6_464 ?
Cl(1) Cl(3) C(19) 99.9(20) . 6_464 ?
Cl(2) Cl(3) C(19) 44.4(19) . 6_464 ?
C(19) Cl(3) C(19) 103.1(42) . 6_464 ?
Cl(2) C(19) Cl(3) 57.2(25) . . ?
Cl(2) C(19) C(18) 38.5(17) . 6_464 ?
Cl(3) C(19) C(18) 18.7(11) . 6_464 ?
Cl(2) C(19) Cl(3) 43.4(19) . 6_464 ?
Cl(3) C(19) Cl(3) 29.9(16) . 6_464 ?
C(18) C(19) Cl(3) 22.9(9) 6_464 6_464 ?
Cl(2) C(19) Cl(2) 38.1(17) . 11_565 ?
Cl(3) C(19) Cl(2) 93.8(32) . 11_565 ?
C(18) C(19) Cl(2) 75.5(23) 6_464 11_565 ?
Cl(3) C(19) Cl(2) 80.5(23) 6_464 11_565 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe N(2) 1.846(3) 15_565 ?
Fe N(2) 1.846(3) . ?
Fe N(1) 1.998(2) 15_565 ?
Fe N(1) 1.998(2) . ?
Fe N(1) 1.998(2) 12_766 ?
Fe N(1) 1.998(2) 6_564 ?
N(1) C(a2) 1.374(3) . ?
N(1) C(a1) 1.379(3) . ?
N(2) O(2) 1.144(11) . ?
N(2) O(2) 1.145(11) 6_564 ?
N(2) O(1) 1.271(4) . ?
N(2) O(1) 1.271(4) 6_564 ?
O(1) O(2) 0.800(10) 6_564 ?
O(1) O(2) 1.518(12) . ?
O(2) O(2) 0.77(2) 6_564 ?
O(2) O(1) 0.800(10) 6_564 ?
C(m1) C(a1) 1.391(3) . ?
C(m1) C(a2) 1.395(3) 15_565 ?
C(m1) C(11) 1.497(3) . ?
C(a1) C(b1) 1.438(3) . ?
C(a2) C(m1) 1.395(3) 12_766 ?
C(a2) C(b2) 1.435(3) . ?
C(b1) C(b2) 1.342(3) . ?
C(11) C(12) 1.386(3) . ?
C(11) C(16) 1.393(3) . ?
C(12) C(13) 1.393(3) . ?
C(13) C(14) 1.377(3) . ?
C(14) O(3) 1.369(3) . ?
C(14) C(15) 1.386(4) . ?
C(15) C(16) 1.387(3) . ?
C(17) O(3) 1.424(4) . ?
Cl(1) Cl(3) 1.329(14) 6_464 ?
Cl(1) Cl(3) 1.329(14) . ?
Cl(1) C(18) 1.501(14) . ?
Cl(1) C(18) 1.501(14) 6_464 ?
Cl(2) C(18) 1.201(13) 6_464 ?
Cl(2) C(18) 1.201(13) . ?
Cl(2) Cl(2) 1.37(2) 11_565 ?
Cl(2) Cl(3) 1.38(2) . ?
Cl(2) Cl(3) 1.38(2) 6_464 ?
Cl(2) C(19) 1.41(6) 6_464 ?
Cl(2) C(19) 1.41(6) . ?
Cl(2) C(19) 2.16(7) 16_665 ?
Cl(2) C(19) 2.17(7) 11_565 ?
Cl(3) C(18) 0.709(14) 6_464 ?
Cl(3) Cl(3) 1.04(3) 6_464 ?
Cl(3) C(19) 1.47(6) . ?
Cl(3) C(19) 2.01(7) 6_464 ?
C(19) C(18) 1.92(7) 6_464 ?
C(19) Cl(3) 2.01(7) 6_464 ?
C(19) Cl(2) 2.17(7) 11_565 ?
