#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:44:58 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258906 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/00/7060027.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_7060027
loop_
_publ_author_name
'Song, Li-Cheng'
'Chen, Wei'
'Zhu, Liang'
'Hu, Fu-Qiang'
'Jiang, Kai-Yu'
_publ_section_title
;
 Synthesis, characterization, and some properties of two types of new
 [Fe]-H2ase models containing a 4-phosphatopyridine or a
 4-phosphatoguanosinepyridine moiety
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18496
_journal_page_last               18507
_journal_paper_doi               10.1039/D0NJ04194G
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C18 H18 Fe N2 O5 S, H2 O'
_chemical_formula_sum            'C18 H20 Fe N2 O6 S'
_chemical_formula_weight         448.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2020-08-17 deposited with the CCDC.	2020-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                94.416(4)
_cell_angle_beta                 100.835(4)
_cell_angle_gamma                107.189(4)
_cell_formula_units_Z            2
_cell_length_a                   8.2237(4)
_cell_length_b                   10.2873(5)
_cell_length_c                   11.9807(5)
_cell_measurement_reflns_used    10014
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0200
_cell_measurement_theta_min      2.6310
_cell_volume                     941.49(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00  65.00   1.00    1.00    --  -25.00  45.00   0.00  180
  2  ω   -115.00  65.00   1.00    1.00    --  -25.00  45.00  90.00  180
  3  ω   -115.00  65.00   1.00    1.00    --  -25.00  45.00 180.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0368216000
_diffrn_orient_matrix_UB_12      -0.0503631000
_diffrn_orient_matrix_UB_13      -0.0173449000
_diffrn_orient_matrix_UB_21      -0.0562764000
_diffrn_orient_matrix_UB_22      -0.0132358000
_diffrn_orient_matrix_UB_23      -0.0551410000
_diffrn_orient_matrix_UB_31      0.0636223000
_diffrn_orient_matrix_UB_32      0.0510235000
_diffrn_orient_matrix_UB_33      -0.0191331000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9296
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         1.748
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0354P)²+0.6065P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3479
_reflns_number_total             3735
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj04194g2.cif
_cod_data_source_block           C
_cod_depositor_comments
'Adding full bibliography for 7060026--7060027.cif.'
_cod_database_code               7060027
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.954
_reflns_odcompleteness_completeness 96.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6B
 0.85 with sigma of 0.005
3.a Free rotating group:
 H6A(H6B)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C18(H18A,H18B,
 H18C)
3.e Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.792
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.65042(3) 0.82864(2) 0.22963(2) 0.01396(9) Uani 1 1 d . . . . .
S1 S 0.93116(5) 0.98375(4) 0.31340(4) 0.01954(11) Uani 1 1 d . . . . .
O1 O 0.30880(18) 0.63389(15) 0.12114(13) 0.0334(3) Uani 1 1 d . . . . .
O2 O 0.56221(17) 1.05474(13) 0.13127(11) 0.0263(3) Uani 1 1 d . . . . .
O3 O 0.44644(17) 0.93287(14) 0.35888(11) 0.0265(3) Uani 1 1 d . . . . .
O4 O 0.78062(18) 0.42077(13) 0.56137(10) 0.0235(3) Uani 1 1 d . . . . .
H4 H 0.802345 0.354614 0.532653 0.035 Uiso 1 1 calc GR . . . .
O5 O 0.75399(15) 0.54858(12) 0.18332(10) 0.0182(3) Uani 1 1 d . . . . .
N1 N 0.70541(17) 0.68282(14) 0.32724(11) 0.0144(3) Uani 1 1 d . . . . .
N2 N 0.81954(18) 0.82579(14) 0.12187(12) 0.0168(3) Uani 1 1 d . . . . .
C1 C 0.4444(2) 0.70886(18) 0.16112(15) 0.0197(4) Uani 1 1 d . . . . .
C2 C 0.5983(2) 0.96521(18) 0.16803(14) 0.0176(3) Uani 1 1 d . . . . .
C3 C 0.5529(2) 0.87223(17) 0.35592(14) 0.0176(3) Uani 1 1 d . . . . .
C4 C 0.6325(2) 0.82644(18) 0.46509(14) 0.0190(3) Uani 1 1 d . . . . .
H4A H 0.732247 0.901422 0.508310 0.023 Uiso 1 1 calc R . . . .
H4B H 0.547280 0.803194 0.512420 0.023 Uiso 1 1 calc R . . . .
C5 C 0.6889(2) 0.70469(17) 0.43772(14) 0.0157(3) Uani 1 1 d . . . . .
C6 C 0.7198(2) 0.62084(17) 0.51825(14) 0.0165(3) Uani 1 1 d . . . . .
C7 C 0.7579(2) 0.50271(17) 0.48152(14) 0.0168(3) Uani 1 1 d . . . . .
C8 C 0.7645(2) 0.47216(17) 0.36723(14) 0.0167(3) Uani 1 1 d . . . . .
C9 C 0.7441(2) 0.56932(17) 0.29529(14) 0.0151(3) Uani 1 1 d . . . . .
C10 C 0.9268(2) 0.5559(2) 0.16771(16) 0.0252(4) Uani 1 1 d . . . . .
H10A H 0.919565 0.520718 0.089712 0.038 Uiso 1 1 calc GR . . . .
H10B H 0.974324 0.501927 0.218515 0.038 Uiso 1 1 calc GR . . . .
H10C H 1.001094 0.649745 0.184546 0.038 Uiso 1 1 calc GR . . . .
C11 C 0.7812(3) 0.33698(18) 0.32282(15) 0.0231(4) Uani 1 1 d . . . . .
H11A H 0.899317 0.337614 0.348608 0.035 Uiso 1 1 calc GR . . . .
H11B H 0.751057 0.323194 0.240434 0.035 Uiso 1 1 calc GR . . . .
H11C H 0.704000 0.263864 0.351086 0.035 Uiso 1 1 calc GR . . . .
C12 C 0.7107(2) 0.65211(19) 0.64123(14) 0.0212(4) Uani 1 1 d . . . . .
H12A H 0.791365 0.741361 0.673547 0.032 Uiso 1 1 calc GR . . . .
H12B H 0.740441 0.584172 0.684129 0.032 Uiso 1 1 calc GR . . . .
H12C H 0.594478 0.650768 0.644488 0.032 Uiso 1 1 calc GR . . . .
C13 C 0.9696(2) 0.91371(17) 0.18709(15) 0.0185(3) Uani 1 1 d . . . . .
C14 C 1.1270(2) 0.9424(2) 0.15137(17) 0.0251(4) Uani 1 1 d . . . . .
H14 H 1.230757 0.999950 0.198372 0.030 Uiso 1 1 calc R . . . .
C15 C 1.1223(3) 0.8817(2) 0.04301(17) 0.0280(4) Uani 1 1 d . . . . .
H15 H 1.224850 0.897617 0.016563 0.034 Uiso 1 1 calc R . . . .
C16 C 0.9667(3) 0.7977(2) -0.02609(16) 0.0261(4) Uani 1 1 d . . . . .
H16 H 0.963791 0.759755 -0.099737 0.031 Uiso 1 1 calc R . . . .
C17 C 0.8143(2) 0.77010(18) 0.01506(15) 0.0203(4) Uani 1 1 d . . . . .
C18 C 0.6416(3) 0.6814(2) -0.05461(15) 0.0256(4) Uani 1 1 d . . . . .
H18A H 0.594088 0.606969 -0.014412 0.038 Uiso 1 1 calc GR . . . .
H18B H 0.655691 0.645187 -0.127171 0.038 Uiso 1 1 calc GR . . . .
H18C H 0.563593 0.734888 -0.067166 0.038 Uiso 1 1 calc GR . . . .
O6 O 0.8306(2) 0.18066(15) 0.53909(13) 0.0302(3) Uani 1 1 d D . . . .
H6A H 0.904095 0.156169 0.564348 0.036 Uiso 1 1 d . . . . .
H6B H 0.745231 0.142638 0.568637 0.036 Uiso 1 1 d DG . . . .
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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 '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
N1 Fe1 S1 89.84(4) . . ?
N1 Fe1 N2 97.48(5) . . ?
N2 Fe1 S1 69.81(4) . . ?
C1 Fe1 S1 176.99(6) . . ?
C1 Fe1 N1 90.08(7) . . ?
C1 Fe1 N2 107.23(7) . . ?
C1 Fe1 C3 89.56(7) . . ?
C2 Fe1 S1 88.09(6) . . ?
C2 Fe1 N1 170.40(6) . . ?
C2 Fe1 N2 90.61(6) . . ?
C2 Fe1 C1 92.47(8) . . ?
C2 Fe1 C3 87.98(7) . . ?
C3 Fe1 S1 93.42(5) . . ?
C3 Fe1 N1 82.78(6) . . ?
C3 Fe1 N2 163.21(7) . . ?
C13 S1 Fe1 79.45(6) . . ?
C9 O5 C10 114.01(13) . . ?
C5 N1 Fe1 113.10(10) . . ?
C9 N1 Fe1 129.40(11) . . ?
C9 N1 C5 117.39(14) . . ?
C13 N2 Fe1 100.45(10) . . ?
C17 N2 Fe1 138.96(12) . . ?
C17 N2 C13 120.50(15) . . ?
O1 C1 Fe1 176.76(16) . . ?
O2 C2 Fe1 177.63(15) . . ?
O3 C3 Fe1 129.11(13) . . ?
O3 C3 C4 119.48(15) . . ?
C4 C3 Fe1 111.35(11) . . ?
C5 C4 C3 110.94(13) . . ?
N1 C5 C4 114.68(14) . . ?
N1 C5 C6 123.16(15) . . ?
C6 C5 C4 122.16(15) . . ?
C5 C6 C7 117.72(15) . . ?
C5 C6 C12 121.95(15) . . ?
C7 C6 C12 120.31(15) . . ?
O4 C7 C6 116.02(15) . . ?
O4 C7 C8 123.30(15) . . ?
C8 C7 C6 120.63(15) . . ?
C7 C8 C11 121.26(15) . . ?
C9 C8 C7 116.70(15) . . ?
C9 C8 C11 121.92(15) . . ?
O5 C9 C8 120.12(14) . . ?
N1 C9 O5 115.73(14) . . ?
N1 C9 C8 124.07(15) . . ?
N2 C13 S1 110.13(12) . . ?
N2 C13 C14 122.00(16) . . ?
C14 C13 S1 127.85(15) . . ?
C15 C14 C13 117.25(18) . . ?
C16 C15 C14 120.58(17) . . ?
C15 C16 C17 119.67(17) . . ?
N2 C17 C16 119.82(17) . . ?
N2 C17 C18 117.41(15) . . ?
C16 C17 C18 122.77(16) . . ?
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 S1 2.3640(5) . ?
Fe1 N1 2.0723(14) . ?
Fe1 N2 2.0726(14) . ?
Fe1 C1 1.7746(18) . ?
Fe1 C2 1.7603(18) . ?
Fe1 C3 1.9230(17) . ?
S1 C13 1.7482(17) . ?
O1 C1 1.141(2) . ?
O2 C2 1.142(2) . ?
O3 C3 1.220(2) . ?
O4 C7 1.346(2) . ?
O5 C9 1.3634(19) . ?
O5 C10 1.449(2) . ?
N1 C5 1.364(2) . ?
N1 C9 1.345(2) . ?
N2 C13 1.349(2) . ?
N2 C17 1.349(2) . ?
C3 C4 1.522(2) . ?
C4 C5 1.493(2) . ?
C5 C6 1.380(2) . ?
C6 C7 1.401(2) . ?
C6 C12 1.504(2) . ?
C7 C8 1.396(2) . ?
C8 C9 1.396(2) . ?
C8 C11 1.504(2) . ?
C13 C14 1.395(2) . ?
C14 C15 1.385(3) . ?
C15 C16 1.381(3) . ?
C16 C17 1.392(3) . ?
C17 C18 1.489(3) . ?
