Hydrophilic quaternary ammonium-group-containing [FeFe]H<sub>2</sub>ase models prepared by quaternization of the pyridyl N atoms in pyridylazadiphosphine- and pyridylmethylazadiphosphine-bridged diiron complexes with various electrophiles.
Song, Li-Cheng; Feng, Li; Guo, Yuan-Qiang; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1443–1453; doi:10.1039/c8dt04211j

data_7048459
_publ_section_title
;
 Hydrophilic quaternary ammonium-group-containing [FeFe]H<sub>2</sub>ase
 models prepared by quaternization of the pyridyl N atoms in
 pyridylazadiphosphine- and pyridylmethylazadiphosphine-bridged diiron
 complexes with various electrophiles.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1443
_journal_page_last               1453
_journal_paper_doi               10.1039/c8dt04211j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C38 H34 Fe2 N2 O8 P2 S3, C H2 Cl2'
_chemical_formula_sum            'C39 H36 Cl2 Fe2 N2 O8 P2 S3'
_chemical_formula_weight         1001.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-15 deposited with the CCDC.
2019-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                77.23(3)
_cell_angle_beta                 79.37(3)
_cell_angle_gamma                69.84(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4838(19)
_cell_length_b                   11.511(2)
_cell_length_c                   21.768(4)
_cell_measurement_reflns_used    5687
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9664
_cell_measurement_theta_min      1.9127
_cell_volume                     2160.3(8)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_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      113.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25114
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.902
_diffrn_reflns_theta_min         1.932
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.249
_refine_diff_density_min         -1.736
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.0075(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         10218
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0878P)^2^+1.4467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1673
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7237
_reflns_number_total             10218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04211j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7048458--7048461.cif.'
_cod_original_cell_volume        2160.4(9)
_cod_database_code               7048459
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.815
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C25, C25'}
3. Uiso/Uaniso restraints and constraints
O5 \\sim O5' \\sim C25 \\sim C25' \\sim C26 \\sim C26': within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O5') \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C25')
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C26') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C25) = Uanis(C25')
4. Others
 Sof(O5')=Sof(C25')=Sof(H25C)=Sof(H25D)=Sof(C26')=Sof(H26C)=Sof(H26D)=1-FVAR(1)
 Sof(O5)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C25(H25A,H25B), C26(H26A,H26B),
 C25'(H25C,H25D), C26'(H26C,H26D), C39(H39A,H39B)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              59755
_olex2_submission_special_instructions 'No special instructions were received'