#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:34:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179067 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/29/4302922.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_4302922
loop_
_publ_author_name
'Ming-Hsi Chiang'
'Yu-Chiao Liu'
'Shu-Ting Yang'
'Gene-Hsiang Lee'
_publ_section_title
;
Biomimetic Model Featuring the NH Proton and Bridging Hydride Related to a
Proposed Intermediate in Enzymatic H2 Production by Fe-Only Hydrogenase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7604
_journal_page_last               7612
_journal_paper_doi               10.1021/ic900564q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C42 H82 B4 F16 Fe4 N6 O8 P4 S4'
_chemical_formula_weight         1621.90
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.990(2)
_cell_angle_beta                 94.040(2)
_cell_angle_gamma                113.709(2)
_cell_formula_units_Z            1
_cell_length_a                   12.0713(5)
_cell_length_b                   12.7630(5)
_cell_length_c                   14.1186(5)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.00
_cell_volume                     1846.32(13)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_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(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω 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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17715
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.236
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.1031
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1962P)²+6.1445P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2985
_refine_ls_wR_factor_ref         0.3227
_reflns_number_gt                4834
_reflns_number_total             6428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900564q_si_003.cif
_cod_data_source_block           ic13337
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 
;
_cod_original_cell_volume        1846.32(12)
_cod_database_code               4302922
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
Fe1 Fe 2.06783(12) 0.85922(10) 1.19587(9) 0.0687(4) Uani 1 1 d . . .
Fe2 Fe 1.93041(11) 0.65697(10) 1.21802(9) 0.0669(4) Uani 1 1 d . . .
H1A H 1.958(9) 0.804(9) 1.252(7) 0.100 Uiso 1 1 d . . .
S1 S 1.95453(19) 0.67531(17) 1.06414(15) 0.0637(5) Uani 1 1 d . . .
S2 S 1.8594(2) 0.25714(18) 0.75155(16) 0.0678(5) Uani 1 1 d . . .
P1 P 2.2175(2) 0.95274(19) 1.12377(17) 0.0699(6) Uani 1 1 d . . .
P2 P 1.9393(3) 0.6823(3) 1.38362(19) 0.0844(7) Uani 1 1 d . . .
O1 O 1.9191(8) 0.9688(7) 1.1351(7) 0.112(3) Uani 1 1 d . . .
O2 O 2.2048(9) 1.0665(7) 1.3902(6) 0.113(3) Uani 1 1 d . . .
O3 O 1.6697(8) 0.6068(9) 1.1868(7) 0.112(3) Uani 1 1 d . . .
O4 O 1.8794(7) 0.3996(6) 1.1584(7) 0.098(2) Uani 1 1 d . . .
N1 N 1.6948(9) 0.4796(9) 0.8409(8) 0.114(4) Uani 1 1 d . . .
H1B H 1.6276 0.4031 0.8255 0.137 Uiso 1 1 calc R . .
C1 C 1.9779(10) 0.9283(8) 1.1596(8) 0.083(2) Uani 1 1 d . . .
C2 C 2.1490(11) 0.9860(9) 1.3151(8) 0.085(3) Uani 1 1 d . . .
C3 C 1.7711(10) 0.6259(9) 1.1983(7) 0.082(3) Uani 1 1 d . . .
C4 C 1.8986(8) 0.4988(8) 1.1809(7) 0.072(2) Uani 1 1 d . . .
C5 C 1.8158(8) 0.6700(8) 0.9968(6) 0.070(2) Uani 1 1 d . . .
H5A H 1.7865 0.7222 1.0454 0.084 Uiso 1 1 calc R . .
H5B H 1.8371 0.7037 0.9426 0.084 Uiso 1 1 calc R . .
C6 C 1.7107(9) 0.5371(9) 0.9486(9) 0.094(3) Uani 1 1 d . . .
H6A H 1.7278 0.4864 0.9827 0.113 Uiso 1 1 calc R . .
H6B H 1.6317 0.5382 0.9623 0.113 Uiso 1 1 calc R . .
C7 C 1.7963(10) 0.4462(9) 0.8110(7) 0.083(3) Uani 1 1 d . . .
H7A H 1.7832 0.4166 0.7356 0.099 Uiso 1 1 calc R . .
H7B H 1.8766 0.5213 0.8395 0.099 Uiso 1 1 calc R . .
C8 C 1.8046(9) 0.3501(8) 0.8459(7) 0.075(2) Uani 1 1 d . . .
H8A H 1.7221 0.2965 0.8531 0.090 Uiso 1 1 calc R . .
H8B H 1.8630 0.3896 0.9133 0.090 Uiso 1 1 calc R . .
C9 C 1.6478(13) 0.5345(14) 0.7872(10) 0.128(4) Uani 1 1 d D . .
H9A H 1.7186 0.6082 0.7862 0.153 Uiso 1 1 calc R . .
H9B H 1.5941 0.5634 0.8264 0.153 Uiso 1 1 calc R . .
C10 C 1.5753(15) 0.4578(16) 0.6798(11) 0.156(6) Uani 1 1 d D . .
H10A H 1.4988 0.3871 0.6781 0.187 Uiso 1 1 calc R . .
H10B H 1.6254 0.4258 0.6381 0.187 Uiso 1 1 calc R . .
C11 C 1.543(2) 0.541(2) 0.639(2) 0.245(14) Uani 1 1 d D . .
H11A H 1.5845 0.5519 0.5830 0.367 Uiso 1 1 calc R . .
H11B H 1.5704 0.6214 0.6937 0.367 Uiso 1 1 calc R . .
H11C H 1.4529 0.5038 0.6134 0.367 Uiso 1 1 calc R . .
C12 C 2.2137(12) 0.8706(11) 0.9945(8) 0.101(3) Uani 1 1 d . . .
H12A H 2.1442 0.8640 0.9488 0.152 Uiso 1 1 calc R . .
H12B H 2.2030 0.7880 0.9871 0.152 Uiso 1 1 calc R . .
H12C H 2.2917 0.9149 0.9769 0.152 Uiso 1 1 calc R . .
C13 C 2.2320(16) 1.0981(12) 1.1268(14) 0.143(6) Uani 1 1 d . . .
H13A H 2.2932 1.1294 1.0880 0.214 Uiso 1 1 calc R . .
H13B H 2.2594 1.1562 1.1978 0.214 Uiso 1 1 calc R . .
H13C H 2.1515 1.0888 1.0964 0.214 Uiso 1 1 calc R . .
C14 C 2.3742(11) 0.9895(14) 1.1847(12) 0.127(5) Uani 1 1 d . . .
H14A H 2.4314 1.0145 1.1412 0.190 Uiso 1 1 calc R . .
H14B H 2.3742 0.9168 1.1945 0.190 Uiso 1 1 calc R . .
H14C H 2.4010 1.0570 1.2512 0.190 Uiso 1 1 calc R . .
C15 C 2.038(2) 0.8447(14) 1.4782(10) 0.156(7) Uani 1 1 d . . .
H15A H 2.0306 0.8475 1.5476 0.234 Uiso 1 1 calc R . .
H15B H 2.0087 0.9005 1.4628 0.234 Uiso 1 1 calc R . .
H15C H 2.1246 0.8705 1.4733 0.234 Uiso 1 1 calc R . .
C16 C 2.0130(17) 0.6084(17) 1.4333(9) 0.139(6) Uani 1 1 d . . .
H16A H 2.0232 0.6366 1.5077 0.209 Uiso 1 1 calc R . .
H16B H 2.0946 0.6290 1.4164 0.209 Uiso 1 1 calc R . .
H16C H 1.9617 0.5191 1.4032 0.209 Uiso 1 1 calc R . .
C17 C 1.7897(16) 0.650(2) 1.4196(11) 0.163(7) Uani 1 1 d . . .
H17A H 1.7246 0.5751 1.3672 0.245 Uiso 1 1 calc R . .
H17B H 1.7704 0.7195 1.4255 0.245 Uiso 1 1 calc R . .
H17C H 1.7939 0.6398 1.4854 0.245 Uiso 1 1 calc R . .
B1 B 1.9372(13) 0.7133(11) 0.7142(9) 0.089(3) Uani 1 1 d . . .
F1 F 2.0545(10) 0.7440(12) 0.6945(8) 0.175(4) Uani 1 1 d . . .
F2 F 1.9439(6) 0.7346(5) 0.8136(4) 0.0923(15) Uani 1 1 d . . .
F3 F 1.9105(10) 0.7938(7) 0.6847(5) 0.135(3) Uani 1 1 d . . .
F4 F 1.8757(9) 0.5966(7) 0.6516(6) 0.138(3) Uani 1 1 d . . .
B2 B 1.5108(9) 1.2523(10) 1.0033(13) 0.138(6) Uiso 1 1 d D . .
F5 F 1.4849(14) 1.1472(11) 1.0162(12) 0.108(4) Uiso 0.50 1 d PD A 1
F6 F 1.6308(9) 1.3209(13) 1.0383(13) 0.106(4) Uiso 0.50 1 d PD A 1
F7 F 1.528(3) 1.253(3) 0.9105(16) 0.208(10) Uiso 0.50 1 d PD A 1
F8 F 1.452(2) 1.316(2) 1.039(2) 0.168(8) Uiso 0.50 1 d PD A 1
F5' F 1.4407(15) 1.1314(11) 0.9663(13) 0.127(5) Uiso 0.50 1 d PD A 2
F6' F 1.4250(14) 1.2863(17) 0.9872(16) 0.129(6) Uiso 0.50 1 d PD A 2
F7' F 1.538(3) 1.314(3) 1.1039(15) 0.227(11) Uiso 0.50 1 d PD A 2
F8' F 1.6221(10) 1.2918(14) 0.9906(13) 0.108(4) Uiso 0.50 1 d PD A 2
N2 N 1.199(2) 1.081(2) 0.641(2) 0.271(12) Uiso 1 1 d D . .
C18 C 1.271(2) 1.076(2) 0.694(2) 0.233(12) Uiso 1 1 d D . .
C19 C 1.292(2) 1.005(2) 0.7533(19) 0.216(10) Uiso 1 1 d D . .
H19A H 1.2251 0.9801 0.7888 0.324 Uiso 1 1 calc R . .
H19B H 1.3718 1.0560 0.8034 0.324 Uiso 1 1 calc R . .
H19C H 1.2948 0.9311 0.7065 0.324 Uiso 1 1 calc R . .
N3 N 1.350(3) 0.713(3) 0.715(2) 0.288(13) Uiso 1 1 d D . .
C20 C 1.344(4) 0.735(4) 0.643(3) 0.33(2) Uiso 1 1 d D . .
C21 C 1.378(3) 0.803(3) 0.572(3) 0.318(19) Uiso 1 1 d D . .
H21A H 1.4447 0.7904 0.5419 0.477 Uiso 1 1 calc R . .
H21B H 1.4070 0.8916 0.6098 0.477 Uiso 1 1 calc R . .
H21C H 1.3056 0.7731 0.5171 0.477 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
C1 Fe1 C2 93.2(4) . . ?
C1 Fe1 P1 90.8(3) . . ?
C2 Fe1 P1 88.8(3) . . ?
C1 Fe1 S2 166.8(3) . 2_967 ?
C2 Fe1 S2 90.5(3) . 2_967 ?
P1 Fe1 S2 102.00(9) . 2_967 ?
C1 Fe1 S1 93.2(3) . . ?
C2 Fe1 S1 168.6(3) . . ?
P1 Fe1 S1 100.53(8) . . ?
S2 Fe1 S1 81.26(8) 2_967 . ?
C1 Fe1 Fe2 111.7(3) . . ?
C2 Fe1 Fe2 113.2(3) . . ?
P1 Fe1 Fe2 146.60(8) . . ?
S2 Fe1 Fe2 55.32(7) 2_967 . ?
S1 Fe1 Fe2 55.64(6) . . ?
C3 Fe2 C4 94.5(4) . . ?
C3 Fe2 P2 91.2(3) . . ?
C4 Fe2 P2 92.9(3) . . ?
C3 Fe2 S2 166.3(3) . 2_967 ?
C4 Fe2 S2 99.0(3) . 2_967 ?
P2 Fe2 S2 90.01(10) . 2_967 ?
C3 Fe2 S1 95.0(3) . . ?
C4 Fe2 S1 97.6(3) . . ?
P2 Fe2 S1 167.32(11) . . ?
S2 Fe2 S1 81.35(8) 2_967 . ?
C3 Fe2 Fe1 111.6(3) . . ?
C4 Fe2 Fe1 142.7(3) . . ?
P2 Fe2 Fe1 111.79(9) . . ?
S2 Fe2 Fe1 55.52(6) 2_967 . ?
S1 Fe2 Fe1 55.59(6) . . ?
C5 S1 Fe1 111.9(3) . . ?
C5 S1 Fe2 111.2(3) . . ?
Fe1 S1 Fe2 68.77(7) . . ?
C8 S2 Fe2 111.8(3) . 2_967 ?
C8 S2 Fe1 116.6(3) . 2_967 ?
Fe2 S2 Fe1 69.16(7) 2_967 2_967 ?
C13 P1 C12 105.3(7) . . ?
C13 P1 C14 102.8(8) . . ?
C12 P1 C14 99.8(7) . . ?
C13 P1 Fe1 114.2(4) . . ?
C12 P1 Fe1 118.0(4) . . ?
C14 P1 Fe1 114.7(4) . . ?
C16 P2 C17 110.0(8) . . ?
C16 P2 C15 97.8(8) . . ?
C17 P2 C15 100.6(9) . . ?
C16 P2 Fe2 117.0(4) . . ?
C17 P2 Fe2 113.6(5) . . ?
C15 P2 Fe2 115.6(5) . . ?
C9 N1 C6 111.0(9) . . ?
C9 N1 C7 120.7(11) . . ?
C6 N1 C7 114.3(8) . . ?
O1 C1 Fe1 178.2(10) . . ?
O2 C2 Fe1 177.4(10) . . ?
O3 C3 Fe2 179.2(10) . . ?
O4 C4 Fe2 179.3(10) . . ?
C6 C5 S1 111.4(6) . . ?
N1 C6 C5 114.7(9) . . ?
C8 C7 N1 114.5(9) . . ?
C7 C8 S2 109.2(6) . . ?
N1 C9 C10 117.7(13) . . ?
C9 C10 C11 106.5(15) . . ?
F4 B1 F2 116.1(9) . . ?
F4 B1 F3 115.0(11) . . ?
F2 B1 F3 112.9(9) . . ?
F4 B1 F1 101.6(10) . . ?
F2 B1 F1 109.7(12) . . ?
F3 B1 F1 99.1(10) . . ?
F8' B2 F8 128.0(16) . . ?
F8' B2 F6' 130.6(15) . . ?
F8 B2 F6' 30.9(13) . . ?
F8' B2 F6 28.5(9) . . ?
F8 B2 F6 110.0(16) . . ?
F6' B2 F6 128.5(14) . . ?
F8' B2 F5 106.0(12) . . ?
F8 B2 F5 120.6(17) . . ?
F6' B2 F5 122.0(13) . . ?
F6 B2 F5 106.7(13) . . ?
F8' B2 F5' 117.4(14) . . ?
F8 B2 F5' 114.1(16) . . ?
F6' B2 F5' 98.7(14) . . ?
F6 B2 F5' 132.6(14) . . ?
F5 B2 F5' 33.8(8) . . ?
F8' B2 F7' 97.3(18) . . ?
F8 B2 F7' 61.8(17) . . ?
F6' B2 F7' 92.6(18) . . ?
F6 B2 F7' 68.9(16) . . ?
F5 B2 F7' 91.6(19) . . ?
F5' B2 F7' 119(2) . . ?
F8' B2 F7 61.9(14) . . ?
F8 B2 F7 111(2) . . ?
F6' B2 F7 85.6(17) . . ?
F6 B2 F7 87.8(16) . . ?
F5 B2 F7 116.0(18) . . ?
F5' B2 F7 92.3(18) . . ?
F7' B2 F7 148(2) . . ?
N2 C18 C19 146(2) . . ?
N3 C20 C21 159(3) . . ?
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
Fe1 C1 1.786(10) . ?
Fe1 C2 1.795(11) . ?
Fe1 P1 2.236(2) . ?
Fe1 S2 2.273(2) 2_967 ?
Fe1 S1 2.281(2) . ?
Fe1 Fe2 2.5770(15) . ?
Fe2 C3 1.782(11) . ?
Fe2 C4 1.786(9) . ?
Fe2 P2 2.248(3) . ?
Fe2 S2 2.268(3) 2_967 ?
Fe2 S1 2.282(2) . ?
S1 C5 1.832(9) . ?
S2 C8 1.843(8) . ?
S2 Fe2 2.268(3) 2_967 ?
S2 Fe1 2.273(2) 2_967 ?
P1 C13 1.778(12) . ?
P1 C12 1.788(10) . ?
P1 C14 1.829(13) . ?
P2 C16 1.778(12) . ?
P2 C17 1.831(14) . ?
P2 C15 1.892(16) . ?
O1 C1 1.124(11) . ?
O2 C2 1.143(12) . ?
O3 C3 1.137(12) . ?
O4 C4 1.124(10) . ?
N1 C9 1.406(17) . ?
N1 C6 1.429(15) . ?
N1 C7 1.497(12) . ?
C5 C6 1.544(13) . ?
C7 C8 1.490(12) . ?
C9 C10 1.494(9) . ?
C10 C11 1.517(10) . ?
B1 F4 1.325(14) . ?
B1 F2 1.334(13) . ?
B1 F3 1.358(14) . ?
B1 F1 1.384(16) . ?
B2 F8' 1.279(9) . ?
B2 F8 1.298(10) . ?
B2 F6' 1.305(9) . ?
B2 F6 1.312(9) . ?
B2 F5 1.323(9) . ?
B2 F5' 1.326(9) . ?
B2 F7' 1.333(10) . ?
B2 F7 1.345(10) . ?
N2 C18 1.145(10) . ?
C18 C19 1.485(10) . ?
N3 C20 1.152(10) . ?
C20 C21 1.497(10) . ?
