#------------------------------------------------------------------------------
#$Date: 2021-11-17 10:29:38 +0200 (Wed, 17 Nov 2021) $
#$Revision: 270714 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/52/1565278.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_1565278
loop_
_publ_author_name
'Agarwal, Tashika'
'Kaur-Ghumaan, Sandeep'
_publ_section_title
;
 Mono- and dinuclear mimics of the [FeFe] hydrogenase enzyme featuring
 bis(monothiolato) and 1,3,5-triaza-7-phosphaadamantane ligands
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119442
_journal_paper_doi               10.1016/j.ica.2020.119442
_journal_volume                  504
_journal_year                    2020
_chemical_formula_moiety         'C25 H26 Fe2 N3 O5 P S2'
_chemical_formula_sum            'C25 H26 Fe2 N3 O5 P S2'
_chemical_formula_weight         655.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 94.273(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3487(8)
_cell_length_b                   20.8705(11)
_cell_length_c                   12.8039(7)
_cell_measurement_reflns_used    5103
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.4580
_cell_measurement_theta_min      2.1920
_cell_volume                     2757.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -59.00  70.00   1.00    8.00    --  -20.00  72.00-108.00  129
  2  ω    -55.00  49.00   1.00    8.00    --  -20.00  72.00-180.00  104
  3  ω    -41.00 -10.00   1.00    8.00    --  -20.00 -72.00 -36.00   31
  4  ω    -69.00 -24.00   1.00    8.00    --  -20.00   0.00 -36.00   45
;
_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      0.0284354000
_diffrn_orient_matrix_UB_12      0.0309362000
_diffrn_orient_matrix_UB_13      0.0033614000
_diffrn_orient_matrix_UB_21      -0.0553799000
_diffrn_orient_matrix_UB_22      0.0129091000
_diffrn_orient_matrix_UB_23      -0.0284517000
_diffrn_orient_matrix_UB_31      -0.0291544000
_diffrn_orient_matrix_UB_32      0.0055733000
_diffrn_orient_matrix_UB_33      0.0475903000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_unetI/netI     0.1912
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21961
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.063
_diffrn_reflns_theta_min         2.202
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         8061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1725
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0331P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1607
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3981
_reflns_number_total             8061
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           2
_cod_database_code               1565278
_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   0.968
_shelx_estimated_absorpt_t_min   0.772
_reflns_odcompleteness_completeness 91.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00E(H00A,H00B), C00F(H00C,H00D), C00G(H00E,H00F), C00L(H00G,H00H), C00S(H00J,
 H00K), C010(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00M(H00M), C00O(H00O), C00Q(H00Q), C00R(H00R), C00U(H00U),
 C00Y(H00Y), C00Z(H00Z)
2.c Idealised Me refined as rotating group:
 C011(H01C,H01D,H01E), C012(H01F,H01G,H01H)
;
_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 1.420
_oxdiff_exptl_absorpt_empirical_full_min 0.692
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Fe01 Fe 0.59149(8) 0.29701(3) 0.80699(5) 0.02132(19) Uani 1 1 d . . . . .
Fe02 Fe 0.43162(8) 0.38738(3) 0.82215(5) 0.0241(2) Uani 1 1 d . . . . .
S003 S 0.61812(14) 0.39557(5) 0.73989(9) 0.0229(3) Uani 1 1 d . . . . .
S004 S 0.40433(14) 0.30642(6) 0.70313(9) 0.0243(3) Uani 1 1 d . . . . .
P005 P 0.51243(15) 0.21535(6) 0.89189(9) 0.0214(3) Uani 1 1 d . . . . .
O006 O 0.7598(4) 0.32154(16) 0.9948(3) 0.0384(11) Uani 1 1 d . . . . .
O007 O 0.7535(4) 0.21787(16) 0.6800(3) 0.0372(10) Uani 1 1 d . . . . .
O008 O 0.5535(4) 0.43340(18) 1.0220(3) 0.0423(11) Uani 1 1 d . . . . .
O009 O 0.2166(5) 0.33372(18) 0.9303(3) 0.0469(12) Uani 1 1 d . . . . .
O00A O 0.2890(4) 0.50009(17) 0.7371(3) 0.0477(12) Uani 1 1 d . . . . .
N00B N 0.5585(5) 0.09059(18) 0.9617(3) 0.0266(10) Uani 1 1 d . . . . .
N00C N 0.3304(4) 0.12192(17) 0.9183(3) 0.0245(10) Uani 1 1 d . . . . .
N00D N 0.4469(5) 0.16302(18) 1.0796(3) 0.0282(11) Uani 1 1 d . . . . .
C00E C 0.6145(5) 0.1422(2) 0.8997(3) 0.0253(12) Uani 1 1 d . . . . .
H00A H 0.624879 0.126309 0.827920 0.030 Uiso 1 1 calc R . . . .
H00B H 0.701587 0.153315 0.931832 0.030 Uiso 1 1 calc R . . . .
C00F C 0.4300(5) 0.0727(2) 0.9153(4) 0.0244(12) Uani 1 1 d . . . . .
H00C H 0.438073 0.060567 0.841310 0.029 Uiso 1 1 calc R . . . .
H00D H 0.400656 0.034263 0.952163 0.029 Uiso 1 1 calc R . . . .
C00G C 0.3563(5) 0.1771(2) 0.8515(3) 0.0255(12) Uani 1 1 d . . . . .
H00E H 0.285771 0.208900 0.855265 0.031 Uiso 1 1 calc R . . . .
H00F H 0.357000 0.162672 0.777910 0.031 Uiso 1 1 calc R . . . .
C00H C 0.6967(5) 0.3118(2) 0.9190(4) 0.0243(12) Uani 1 1 d . . . . .
C00I C 0.4280(5) 0.3878(2) 0.5294(4) 0.0277(13) Uani 1 1 d . . . . .
H00I H 0.399588 0.421951 0.571001 0.033 Uiso 1 1 calc R . . . .
C00J C 0.7438(6) 0.4434(2) 0.8016(3) 0.0240(12) Uani 1 1 d . . . . .
C00K C 0.4422(5) 0.3269(2) 0.5712(3) 0.0232(12) Uani 1 1 d . . . . .
C00L C 0.5437(6) 0.1123(2) 1.0697(3) 0.0292(14) Uani 1 1 d . . . . .
H00G H 0.519485 0.074947 1.111853 0.035 Uiso 1 1 calc R . . . .
H00H H 0.628640 0.128006 1.100021 0.035 Uiso 1 1 calc R . . . .
C00M C 0.8712(6) 0.4241(2) 0.8018(4) 0.0268(12) Uani 1 1 d . . . . .
H00M H 0.890306 0.381926 0.779532 0.032 Uiso 1 1 calc R . . . .
C00N C 0.6910(6) 0.2489(2) 0.7312(4) 0.0274(13) Uani 1 1 d . . . . .
C00O C 0.8207(7) 0.5459(2) 0.8687(4) 0.0362(16) Uani 1 1 d . . . . .
H00O H 0.801725 0.587875 0.892037 0.043 Uiso 1 1 calc R . . . .
C00P C 0.9478(7) 0.5270(2) 0.8672(4) 0.0331(15) Uani 1 1 d . . . . .
C00Q C 0.7201(6) 0.5052(2) 0.8370(4) 0.0351(15) Uani 1 1 d . . . . .
H00Q H 0.633207 0.519534 0.839389 0.042 Uiso 1 1 calc R . . . .
C00R C 0.4557(6) 0.3988(2) 0.4261(4) 0.0324(14) Uani 1 1 d . . . . .
H00R H 0.447721 0.440934 0.398105 0.039 Uiso 1 1 calc R . . . .
C00S C 0.4903(6) 0.2230(2) 1.0339(3) 0.0266(13) Uani 1 1 d . . . . .
H00J H 0.573445 0.236219 1.071009 0.032 Uiso 1 1 calc R . . . .
H00K H 0.425799 0.256993 1.044386 0.032 Uiso 1 1 calc R . . . .
C00T C 0.3018(6) 0.3540(2) 0.8874(4) 0.0321(14) Uani 1 1 d . . . . .
C00U C 0.9720(6) 0.4649(3) 0.8338(3) 0.0318(13) Uani 1 1 d . . . . .
H00U H 1.058880 0.450372 0.832968 0.038 Uiso 1 1 calc R . . . .
C00V C 0.4945(6) 0.3493(2) 0.3636(4) 0.0294(13) Uani 1 1 d . . . . .
C00W C 0.3451(6) 0.4569(2) 0.7693(4) 0.0304(13) Uani 1 1 d . . . . .
C00X C 0.5074(6) 0.4163(2) 0.9436(4) 0.0306(14) Uani 1 1 d . . . . .
C00Y C 0.4812(6) 0.2776(2) 0.5093(4) 0.0309(13) Uani 1 1 d . . . . .
H00Y H 0.491376 0.235755 0.537920 0.037 Uiso 1 1 calc R . . . .
C00Z C 0.5055(6) 0.2882(2) 0.4065(4) 0.0297(13) Uani 1 1 d . . . . .
H00Z H 0.530011 0.253384 0.364421 0.036 Uiso 1 1 calc R . . . .
C010 C 0.3232(6) 0.1416(2) 1.0275(3) 0.0283(13) Uani 1 1 d . . . . .
H01A H 0.290543 0.105107 1.067352 0.034 Uiso 1 1 calc R . . . .
H01B H 0.259487 0.176862 1.029950 0.034 Uiso 1 1 calc R . . . .
C011 C 0.5266(6) 0.3611(3) 0.2512(4) 0.0405(16) Uani 1 1 d . . . . .
H01C H 0.450998 0.379508 0.211351 0.061 Uiso 1 1 calc GR . . . .
H01D H 0.549991 0.320497 0.219197 0.061 Uiso 1 1 calc GR . . . .
H01E H 0.599640 0.391021 0.250575 0.061 Uiso 1 1 calc GR . . . .
C012 C 1.0568(7) 0.5722(3) 0.9010(4) 0.053(2) Uani 1 1 d . . . . .
H01F H 1.025466 0.616473 0.895757 0.080 Uiso 1 1 calc GR . . . .
H01G H 1.128007 0.566495 0.855512 0.080 Uiso 1 1 calc GR . . . .
H01H H 1.087665 0.562940 0.973628 0.080 Uiso 1 1 calc GR . . . .
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'
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'
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
S003 Fe01 Fe02 56.44(4) . .
S003 Fe01 S004 79.70(5) . .
S004 Fe01 Fe02 56.39(4) . .
P005 Fe01 Fe02 105.63(5) . .
P005 Fe01 S003 162.01(6) . .
P005 Fe01 S004 91.37(6) . .
C00H Fe01 Fe02 100.07(16) . .
C00H Fe01 S003 93.70(15) . .
C00H Fe01 S004 155.25(17) . .
C00H Fe01 P005 87.93(16) . .
C00H Fe01 C00N 101.3(2) . .
C00N Fe01 Fe02 150.84(15) . .
C00N Fe01 S003 102.42(16) . .
C00N Fe01 S004 103.45(17) . .
C00N Fe01 P005 94.80(16) . .
S003 Fe02 Fe01 55.73(4) . .
S003 Fe02 S004 79.22(5) . .
S004 Fe02 Fe01 56.23(4) . .
C00T Fe02 Fe01 105.40(17) . .
C00T Fe02 S003 160.97(17) . .
C00T Fe02 S004 87.88(16) . .
C00T Fe02 C00W 96.9(3) . .
C00T Fe02 C00X 91.2(2) . .
C00W Fe02 Fe01 151.48(17) . .
C00W Fe02 S003 100.37(18) . .
C00W Fe02 S004 108.13(17) . .
C00X Fe02 Fe01 94.10(17) . .
C00X Fe02 S003 92.58(19) . .
C00X Fe02 S004 148.64(16) . .
C00X Fe02 C00W 103.1(2) . .
Fe01 S003 Fe02 67.83(4) . .
C00J S003 Fe01 116.70(16) . .
C00J S003 Fe02 117.06(17) . .
Fe01 S004 Fe02 67.38(4) . .
C00K S004 Fe01 109.36(18) . .
C00K S004 Fe02 115.06(16) . .
C00E P005 Fe01 115.50(17) . .
C00E P005 C00S 97.4(2) . .
C00G P005 Fe01 123.05(15) . .
C00G P005 C00E 98.2(2) . .
C00G P005 C00S 98.2(2) . .
C00S P005 Fe01 119.49(16) . .
C00F N00B C00E 110.3(4) . .
C00F N00B C00L 107.7(4) . .
C00L N00B C00E 110.6(4) . .
C00F N00C C00G 112.1(4) . .
C00F N00C C010 108.0(4) . .
C010 N00C C00G 111.1(4) . .
C00S N00D C00L 110.5(4) . .
C00S N00D C010 111.2(4) . .
C010 N00D C00L 108.6(4) . .
N00B C00E P005 112.5(4) . .
N00C C00F N00B 115.6(4) . .
N00C C00G P005 111.7(4) . .
O006 C00H Fe01 176.6(5) . .
C00K C00I C00R 119.8(5) . .
C00M C00J S003 120.3(4) . .
C00M C00J C00Q 117.4(5) . .
C00Q C00J S003 121.5(5) . .
C00I C00K S004 123.6(4) . .
C00Y C00K S004 116.9(4) . .
C00Y C00K C00I 119.4(4) . .
N00D C00L N00B 114.9(4) . .
C00J C00M C00U 121.3(5) . .
O007 C00N Fe01 178.3(5) . .
C00P C00O C00Q 121.4(5) . .
C00O C00P C00U 117.7(5) . .
C00O C00P C012 120.8(5) . .
C00U C00P C012 121.5(6) . .
C00O C00Q C00J 121.2(6) . .
C00V C00R C00I 120.9(5) . .
N00D C00S P005 112.4(3) . .
O009 C00T Fe02 178.4(5) . .
C00M C00U C00P 121.0(6) . .
C00R C00V C00Z 118.4(4) . .
C00R C00V C011 121.3(5) . .
C00Z C00V C011 120.3(5) . .
O00A C00W Fe02 178.7(5) . .
O008 C00X Fe02 178.1(5) . .
C00Z C00Y C00K 120.8(5) . .
C00Y C00Z C00V 120.7(5) . .
N00C C010 N00D 114.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe01 Fe02 2.5260(10) .
Fe01 S003 2.2540(13) .
Fe01 S004 2.2748(16) .
Fe01 P005 2.2108(14) .
Fe01 C00H 1.762(5) .
Fe01 C00N 1.778(5) .
Fe02 S003 2.2729(16) .
Fe02 S004 2.2789(13) .
Fe02 C00T 1.777(6) .
Fe02 C00W 1.809(5) .
Fe02 C00X 1.794(6) .
S003 C00J 1.777(5) .
S004 C00K 1.813(5) .
P005 C00E 1.855(5) .
P005 C00G 1.842(5) .
P005 C00S 1.857(4) .
O006 C00H 1.146(5) .
O007 C00N 1.153(6) .
O008 C00X 1.136(6) .
O009 C00T 1.153(6) .
O00A C00W 1.134(6) .
N00B C00E 1.482(6) .
N00B C00F 1.464(6) .
N00B C00L 1.474(5) .
N00C C00F 1.458(6) .
N00C C00G 1.471(5) .
N00C C010 1.465(5) .
N00D C00L 1.470(6) .
N00D C00S 1.467(6) .
N00D C010 1.468(7) .
C00I C00K 1.382(6) .
C00I C00R 1.394(6) .
C00J C00M 1.379(7) .
C00J C00Q 1.395(6) .
C00K C00Y 1.378(6) .
C00M C00U 1.385(7) .
C00O C00P 1.374(8) .
C00O C00Q 1.382(7) .
C00P C00U 1.394(7) .
C00P C012 1.508(8) .
C00R C00V 1.384(7) .
C00V C00Z 1.391(6) .
C00V C011 1.521(6) .
C00Y C00Z 1.376(6) .
