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_1565277
_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         'C20 H14 Fe2 O6 S2'
_chemical_formula_sum            'C20 H14 Fe2 O6 S2'
_chemical_formula_weight         526.13
_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   geom
_cell_angle_alpha                105.228(4)
_cell_angle_beta                 103.008(3)
_cell_angle_gamma                100.239(3)
_cell_formula_units_Z            4
_cell_length_a                   12.3222(4)
_cell_length_b                   13.9057(6)
_cell_length_c                   14.1617(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2207.70(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.871
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32657
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.507
_diffrn_reflns_theta_min         3.324
_exptl_absorpt_coefficient_mu    1.536
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             1064
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         10720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0482
_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/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7455
_reflns_number_total             10720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           1
_cod_original_cell_volume        2207.70(15)
_cod_database_code               1565277
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C01J(H01M,H01N,H01O), C01M(H01P,H01Q,H01R), C01N(H01A,H01B,H01C), C01O(H01E,
 H01F,H01J)
2.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00X(H00X), C00Z(H00Z),
 C010(H010), C016(H016), C017(H017), C019(H019), C01D(H01D), C01G(H01G),
 C01H(H01H), C01I(H01I), C01K(H01K), C01L(H01L)
;
_shelx_res_checksum              55239
_shelx_hkl_checksum              31147
_olex2_submission_special_instructions 'No special instructions were received'