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_7048461
_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
'Br, C40 H39 Fe2 N2 O5 P2 S2, 1.75(C H Cl3), 0.75(C H2 Cl2)'
_chemical_formula_sum            'C42.5 H42.25 Br Cl6.75 Fe2 N2 O5 P2 S2'
_chemical_formula_weight         1217.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 107.058(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1716(6)
_cell_length_b                   29.8239(16)
_cell_length_c                   16.4070(9)
_cell_measurement_reflns_used    6559
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0440
_cell_measurement_theta_min      2.0460
_cell_volume                     5226.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     57.00  93.00   1.00    8.69    --   11.08 178.00 120.00   36
  2  \w    -28.00  92.00   1.00    8.69    --   11.08   0.00-180.00  120
  3  \w    -14.00  25.00   1.00    8.69    --  -11.24 -99.00 120.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0141970000
_diffrn_orient_matrix_UB_12      0.0109975000
_diffrn_orient_matrix_UB_13      0.0343600000
_diffrn_orient_matrix_UB_21      -0.0053536000
_diffrn_orient_matrix_UB_22      0.0206912000
_diffrn_orient_matrix_UB_23      -0.0221092000
_diffrn_orient_matrix_UB_31      -0.0646433000
_diffrn_orient_matrix_UB_32      -0.0041433000
_diffrn_orient_matrix_UB_33      -0.0193538000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24222
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.082
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.849
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.450
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9191
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0604P)^2^+14.9600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7136
_reflns_number_total             9191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04211j2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7048458--7048461.cif.'
_cod_original_formula_sum        'C42.50 H42.25 Br Cl6.75 Fe2 N2 O5 P2 S2'
_cod_database_code               7048461
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.95
_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
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl12) \\sim Ueq, Uanis(Cl8) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: Cl8(0.75) Cl9(0.75) Cl10(0.75) C46(0.75) H46(0.75) Cl11(0.75)
 Cl12(0.75) C47(0.75) H47A(0.75) H47B(0.75)
4.a Ternary CH refined with riding coordinates:
 C45(H45), C46(H46)
4.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C36(H36A,H36B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C47(H47A,H47B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39),
 C40(H40), C41(H41)
4.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              87471
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.213
_oxdiff_exptl_absorpt_empirical_full_min 0.862