Mono- and dinuclear mimics of the [FeFe] hydrogenase enzyme featuring bis(monothiolato) and 1,3,5-triaza-7-phosphaadamantane ligands
Agarwal, Tashika; Kaur-Ghumaan, Sandeep; Inorganica Chimica Acta 504 (2020) 119442–; doi:10.1016/j.ica.2020.119442

data_1565278
_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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -59.00  70.00   1.00    8.00    --  -20.00  72.00-108.00  129
  2  \w    -55.00  49.00   1.00    8.00    --  -20.00  72.00-180.00  104
  3  \w    -41.00 -10.00   1.00    8.00    --  -20.00 -72.00 -36.00   31
  4  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0331P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           2
_cod_database_code               1565278
_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)
;
_shelx_res_checksum              6190
_shelx_hkl_checksum              1135
_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