#------------------------------------------------------------------------------
#$Date: 2018-01-18 09:59:41 +0200 (Thu, 18 Jan 2018) $
#$Revision: 205355 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/87/1548713.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_1548713
loop_
_publ_author_name
'Ming Li'
'Allen G. Oliver'
'Teresa J. Neal'
'Charles E. Schulz'
'W. Robert Scheidt'
_publ_section_title
;
 Effect of the Ruffled Porphyrin Ring on Electronic Structures: Structure
 and Characterization of [Fe(TalkylP)(OClO3)] and [Fe(TPrP)(THF)2]ClO4
 (alkyl = Ethyl, Et and n-Propyl, Pr)
;
_journal_name_full               'Journal of Porphyrins and Phthalocyanines'
_journal_page_first              118
_journal_page_last               124
_journal_paper_doi               10.1142/S1088424612501362
_journal_volume                  17
_journal_year                    2013
_chemical_formula_moiety         'C28 H28 Cl Fe N4 O4'
_chemical_formula_sum            'C28 H28 Cl Fe N4 O4'
_chemical_formula_weight         575.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                111.095(12)
_cell_angle_beta                 96.075(8)
_cell_angle_gamma                105.626(7)
_cell_formula_units_Z            2
_cell_length_a                   10.2565(4)
_cell_length_b                   10.9066(9)
_cell_length_c                   12.5276(13)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      2.35
_cell_volume                     1226.7(2)
_computing_cell_refinement       madnes
_computing_data_collection       madnes
_computing_data_reduction        'Madnes (messerschmitt & Pflugraph, 1987)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 9.23
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  '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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11760
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.83
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangle
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.589
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0471
_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)+(0.0768P)²+1.3073P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                5656
_reflns_number_total             6191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            NIHMS432021-supplement-cif1.cif
_cod_data_source_block           fetetclo4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1548713
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_assembly
_atom_site_disorder_group
Fe(1 Fe 0.91686(3) 0.23847(3) 0.32791(2) 0.01131(9) Uani 1 1 d . . .
N(1) N 0.80684(17) 0.35362(17) 0.40571(14) 0.0143(3) Uani 1 1 d . . .
N(2) N 1.00122(17) 0.25110(17) 0.48221(14) 0.0129(3) Uani 1 1 d . . .
N(3) N 1.06855(17) 0.17852(17) 0.26442(14) 0.0129(3) Uani 1 1 d . . .
N(4) N 0.85925(18) 0.25986(18) 0.18259(14) 0.0146(3) Uani 1 1 d . . .
C(A1 C 0.7053(2) 0.3856(2) 0.35012(18) 0.0166(4) Uani 1 1 d . . .
C(A2 C 0.8097(2) 0.4128(2) 0.52477(17) 0.0148(3) Uani 1 1 d . . .
C(A3 C 0.9669(2) 0.3095(2) 0.58897(16) 0.0146(3) Uani 1 1 d . . .
C(A4 C 1.0881(2) 0.1794(2) 0.50112(17) 0.0150(3) Uani 1 1 d . . .
C(A5 C 1.1593(2) 0.1317(2) 0.31620(17) 0.0153(4) Uani 1 1 d . . .
C(A6 C 1.1030(2) 0.16849(19) 0.15802(16) 0.0143(3) Uani 1 1 d . . .
C(A7 C 0.9096(2) 0.2232(2) 0.08112(16) 0.0164(4) Uani 1 1 d . . .
C(A8 C 0.7401(2) 0.2880(2) 0.15273(17) 0.0170(4) Uani 1 1 d . . .
C(B1 C 0.6484(2) 0.4701(2) 0.4356(2) 0.0215(4) Uani 1 1 d . . .
H(B1 H 0.5776 0.5065 0.4201 0.026 Uiso 1 1 calc R . .
C(B2 C 0.7143(2) 0.4887(2) 0.54293(19) 0.0204(4) Uani 1 1 d . . .
H(B2 H 0.6997 0.5422 0.6165 0.025 Uiso 1 1 calc R . .
C(B3 C 1.0315(2) 0.2714(2) 0.67326(18) 0.0205(4) Uani 1 1 d . . .
H(B3 H 1.0253 0.2991 0.7531 0.025 Uiso 1 1 calc R . .
C(B4 C 1.1032(2) 0.1889(2) 0.61917(18) 0.0197(4) Uani 1 1 d . . .
H(B4 H 1.1538 0.1456 0.6530 0.024 Uiso 1 1 calc R . .
C(B5 C 1.2543(2) 0.0977(2) 0.24364(18) 0.0190(4) Uani 1 1 d . . .
H(B5 H 1.3272 0.0643 0.2599 0.023 Uiso 1 1 calc R . .
C(B6 C 1.2206(2) 0.1221(2) 0.14746(18) 0.0194(4) Uani 1 1 d . . .
H(B6 H 1.2668 0.1106 0.0845 0.023 Uiso 1 1 calc R . .
C(B7 C 0.8198(2) 0.2292(2) -0.01129(18) 0.0220(4) Uani 1 1 d . . .
H(B7 H 0.8324 0.2109 -0.0889 0.026 Uiso 1 1 calc R . .
C(B8 C 0.7140(2) 0.2655(2) 0.03166(19) 0.0233(4) Uani 1 1 d . . .
H(B8 H 0.6369 0.2743 -0.0106 0.028 Uiso 1 1 calc R . .
C(M1 C 0.6635(2) 0.3448(2) 0.22962(18) 0.0173(4) Uani 1 1 d . . .
C(M2 C 0.8822(2) 0.3913(2) 0.61243(16) 0.0156(4) Uani 1 1 d . . .
C(M3 C 1.1624(2) 0.1198(2) 0.42328(17) 0.0152(3) Uani 1 1 d . . .
C(M4 C 1.0279(2) 0.1869(2) 0.06926(16) 0.0159(4) Uani 1 1 d . . .
C(11 C 0.5376(2) 0.3723(2) 0.1813(2) 0.0209(4) Uani 1 1 d . . .
H(1A H 0.4730 0.3733 0.2348 0.025 Uiso 1 1 calc R . .
H(1B H 0.4886 0.2953 0.1040 0.025 Uiso 1 1 calc R . .
C(12 C 0.5746(3) 0.5096(2) 0.1670(2) 0.0271(5) Uani 1 1 d . . .
H(1C H 0.6235 0.5864 0.2432 0.041 Uiso 1 1 calc R . .
H(1D H 0.4895 0.5231 0.1377 0.041 Uiso 1 1 calc R . .
H(1E H 0.6348 0.5076 0.1110 0.041 Uiso 1 1 calc R . .
C(21 C 0.8596(2) 0.4490(2) 0.73571(17) 0.0187(4) Uani 1 1 d . . .
H(2A H 0.8426 0.5383 0.7513 0.022 Uiso 1 1 calc R . .
H(2B H 0.9448 0.4679 0.7927 0.022 Uiso 1 1 calc R . .
C(22 C 0.7367(2) 0.3486(3) 0.75414(19) 0.0250(4) Uani 1 1 d . . .
H(2C H 0.6513 0.3332 0.7006 0.038 Uiso 1 1 calc R . .
H(2D H 0.7274 0.3887 0.8355 0.038 Uiso 1 1 calc R . .
H(2E H 0.7526 0.2597 0.7382 0.038 Uiso 1 1 calc R . .
C(31 C 1.2595(2) 0.0520(2) 0.45976(19) 0.0203(4) Uani 1 1 d . . .
H(3A H 1.2639 -0.0247 0.3892 0.024 Uiso 1 1 calc R . .
H(3B H 1.2212 0.0111 0.5133 0.024 Uiso 1 1 calc R . .
C(32 C 1.4064(2) 0.1536(3) 0.5211(2) 0.0271(5) Uani 1 1 d . . .
H(3C H 1.4473 0.1900 0.4669 0.041 Uiso 1 1 calc R . .
H(3D H 1.4634 0.1051 0.5455 0.041 Uiso 1 1 calc R . .
H(3E H 1.4028 0.2308 0.5903 0.041 Uiso 1 1 calc R . .
C(41 C 1.0811(2) 0.1709(2) -0.04170(17) 0.0197(4) Uani 1 1 d . . .
H(4A H 1.0014 0.1365 -0.1089 0.024 Uiso 1 1 calc R . .
H(4B H 1.1289 0.1007 -0.0571 0.024 Uiso 1 1 calc R . .
C(42 C 1.1810(3) 0.3074(3) -0.0324(2) 0.0263(5) Uani 1 1 d . . .
H(4C H 1.1324 0.3754 -0.0221 0.040 Uiso 1 1 calc R . .
H(4D H 1.2160 0.2918 -0.1043 0.040 Uiso 1 1 calc R . .
H(4E H 1.2590 0.3429 0.0352 0.040 Uiso 1 1 calc R . .
Cl(1 Cl 0.63626(5) -0.03437(5) 0.20952(4) 0.01708(12) Uani 1 1 d . . .
O(1) O 0.78188(15) 0.03721(16) 0.28103(13) 0.0192(3) Uani 1 1 d . . .
O(2) O 0.5519(2) 0.0397(2) 0.2664(2) 0.0457(6) Uani 1 1 d . . .
O(3) O 0.6349(2) -0.0351(2) 0.09567(15) 0.0364(4) Uani 1 1 d . . .
O(4) O 0.59571(19) -0.17262(19) 0.20328(18) 0.0334(4) Uani 1 1 d . . .
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
N(4) Fe(1 N(2) 169.33(7) . .
N(4) Fe(1 N(1) 89.40(7) . .
N(2) Fe(1 N(1) 89.27(7) . .
N(4) Fe(1 N(3) 89.07(7) . .
N(2) Fe(1 N(3) 89.09(7) . .
N(1) Fe(1 N(3) 162.94(7) . .
N(4) Fe(1 O(1) 98.13(7) . .
N(2) Fe(1 O(1) 92.50(6) . .
N(1) Fe(1 O(1) 102.01(7) . .
N(3) Fe(1 O(1) 95.03(6) . .
C(A1 N(1) C(A2 105.87(16) . .
C(A1 N(1) Fe(1 126.08(13) . .
C(A2 N(1) Fe(1 127.99(13) . .
C(A3 N(2) C(A4 105.56(16) . .
C(A3 N(2) Fe(1 127.68(13) . .
C(A4 N(2) Fe(1 125.72(13) . .
C(A5 N(3) C(A6 105.57(16) . .
C(A5 N(3) Fe(1 126.32(13) . .
C(A6 N(3) Fe(1 128.06(13) . .
C(A8 N(4) C(A7 105.39(16) . .
C(A8 N(4) Fe(1 125.31(13) . .
C(A7 N(4) Fe(1 128.09(14) . .
N(1) C(A1 C(M1 126.27(18) . .
N(1) C(A1 C(B1 109.76(18) . .
C(M1 C(A1 C(B1 123.96(19) . .
C(M2 C(A2 N(1) 125.98(18) . .
C(M2 C(A2 C(B2 124.14(18) . .
N(1) C(A2 C(B2 109.57(17) . .
C(M2 C(A3 N(2) 126.27(18) . .
C(M2 C(A3 C(B3 124.13(18) . .
N(2) C(A3 C(B3 109.60(17) . .
C(M3 C(A4 N(2) 125.83(18) . .
C(M3 C(A4 C(B4 123.86(18) . .
N(2) C(A4 C(B4 109.96(17) . .
N(3) C(A5 C(M3 126.51(17) . .
N(3) C(A5 C(B5 109.93(18) . .
C(M3 C(A5 C(B5 123.56(18) . .
N(3) C(A6 C(M4 125.86(18) . .
N(3) C(A6 C(B6 109.71(17) . .
C(M4 C(A6 C(B6 124.16(18) . .
C(M4 C(A7 N(4) 126.08(18) . .
C(M4 C(A7 C(B7 124.39(18) . .
N(4) C(A7 C(B7 109.52(18) . .
N(4) C(A8 C(M1 126.05(18) . .
N(4) C(A8 C(B8 110.34(18) . .
C(M1 C(A8 C(B8 123.25(19) . .
C(B2 C(B1 C(A1 107.32(18) . .
C(B1 C(B2 C(A2 107.38(18) . .
C(B4 C(B3 C(A3 107.89(18) . .
C(B3 C(B4 C(A4 106.92(18) . .
C(B6 C(B5 C(A5 107.17(18) . .
C(B5 C(B6 C(A6 107.53(18) . .
C(B8 C(B7 C(A7 107.79(18) . .
C(B7 C(B8 C(A8 106.89(19) . .
C(A8 C(M1 C(A1 121.46(19) . .
C(A8 C(M1 C(11 118.65(18) . .
C(A1 C(M1 C(11 119.72(18) . .
C(A2 C(M2 C(A3 121.95(18) . .
C(A2 C(M2 C(21 119.18(18) . .
C(A3 C(M2 C(21 118.69(18) . .
C(A4 C(M3 C(A5 121.39(18) . .
C(A4 C(M3 C(31 119.50(18) . .
C(A5 C(M3 C(31 118.86(18) . .
C(A7 C(M4 C(A6 121.88(18) . .
C(A7 C(M4 C(41 119.59(18) . .
C(A6 C(M4 C(41 118.51(18) . .
C(M1 C(11 C(12 113.04(18) . .
C(M2 C(21 C(22 112.18(17) . .
C(M3 C(31 C(32 113.04(18) . .
C(M4 C(41 C(42 111.98(17) . .
O(2) Cl(1 O(3) 111.04(14) . .
O(2) Cl(1 O(4) 111.60(14) . .
O(3) Cl(1 O(4) 110.68(12) . .
O(2) Cl(1 O(1) 108.15(11) . .
O(3) Cl(1 O(1) 108.38(11) . .
O(4) Cl(1 O(1) 106.81(10) . .
Cl(1 O(1) Fe(1 130.89(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe(1 N(4) 1.9672(16) .
Fe(1 N(2) 1.9734(16) .
Fe(1 N(1) 1.9787(17) .
Fe(1 N(3) 1.9790(16) .
Fe(1 O(1) 2.0839(15) .
N(1) C(A1 1.382(2) .
N(1) C(A2 1.389(2) .
N(2) C(A3 1.387(2) .
N(2) C(A4 1.388(2) .
N(3) C(A5 1.384(2) .
N(3) C(A6 1.389(2) .
N(4) C(A8 1.385(3) .
N(4) C(A7 1.388(2) .
C(A1 C(M1 1.392(3) .
C(A1 C(B1 1.431(3) .
C(A2 C(M2 1.386(3) .
C(A2 C(B2 1.429(3) .
C(A3 C(M2 1.386(3) .
C(A3 C(B3 1.429(3) .
C(A4 C(M3 1.386(3) .
C(A4 C(B4 1.433(3) .
C(A5 C(M3 1.391(3) .
C(A5 C(B5 1.433(3) .
C(A6 C(M4 1.391(3) .
C(A6 C(B6 1.429(3) .
C(A7 C(M4 1.381(3) .
C(A7 C(B7 1.433(3) .
C(A8 C(M1 1.386(3) .
C(A8 C(B8 1.429(3) .
C(B1 C(B2 1.358(3) .
C(B3 C(B4 1.353(3) .
C(B5 C(B6 1.354(3) .
C(B7 C(B8 1.352(3) .
C(M1 C(11 1.516(3) .
C(M2 C(21 1.513(3) .
C(M3 C(31 1.514(3) .
C(M4 C(41 1.516(3) .
C(11 C(12 1.522(3) .
C(21 C(22 1.530(3) .
C(31 C(32 1.527(3) .
C(41 C(42 1.519(3) .
Cl(1 O(2) 1.4149(19) .
Cl(1 O(3) 1.4219(18) .
Cl(1 O(4) 1.4224(18) .
Cl(1 O(1) 1.4927(15) .
