Functionalized nickel(II)-iron(II) dithiolates as biomimetic models of [NiFe]-H2ases
Song, Li-Cheng; Wang, Yin-Peng; Dong, Yi-Xiong; Yang, Xi-Yue; Dalton Transactions  (2023) –; doi:10.1039/D3DT00039G

data_7712286
_publ_section_title
;
 Functionalized nickel(II)-iron(II) dithiolates as biomimetic models of
 [NiFe]-H2ases
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00039G
_journal_year                    2023
_chemical_formula_sum            'C129 H120 Cl6 F24 Fe2 N2 Ni2 O4 P12 S4'
_chemical_formula_weight         3159.96
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.98(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.641(5)
_cell_length_b                   22.520(5)
_cell_length_c                   27.283(6)
_cell_measurement_reflns_used    30617
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.9745
_cell_measurement_theta_min      1.4278
_cell_volume                     13808(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2018)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Saturn70 (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            166584
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.952
_diffrn_reflns_theta_min         1.280
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7459
_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            'clear light red'
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             6440
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1709
_refine_ls_number_reflns         33026
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0927P)^2^+17.6461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1802
_refine_ls_wR_factor_ref         0.1969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25590
_reflns_number_total             33026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00039g2.cif
_cod_data_source_block           r20181030c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7712286
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.958
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C129-Cl5 = C129-Cl6 = C130-Cl5' = C130-Cl6'
 1.72 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C40) \\sim Ueq, Uanis(C40A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C39A) = Uanis(C39)
Uanis(F8) = Uanis(F8A)
Uanis(F10A) = Uanis(F10)
Uanis(F9) = Uanis(F9A)
Uanis(C129) = Uanis(C130)
Uanis(Cl5) = Uanis(Cl5')
Uanis(Cl6) = Uanis(Cl6')
Uanis(C59) = Uanis(C59')
Uanis(C60) = Uanis(C60')
Uanis(C61) = Uanis(C61')
Uanis(C62) = Uanis(C62')
Uanis(C63) = Uanis(C63')
4. Others
 Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(H41A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=
 Sof(H40A)=1-FVAR(1)
 Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=
 Sof(H41)=FVAR(1)
 Sof(Cl5')=Sof(Cl6')=Sof(C130)=Sof(H13A)=Sof(H13B)=1-FVAR(2)
 Sof(Cl5)=Sof(Cl6)=Sof(C129)=Sof(H12E)=Sof(H12F)=FVAR(2)
 Sof(C59')=Sof(H59')=Sof(C60')=Sof(H60')=Sof(C61')=Sof(H61')=Sof(C62')=
 Sof(H62')=Sof(C63')=Sof(H63')=1-FVAR(3)
 Sof(C59)=Sof(H59)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=
 Sof(C63)=Sof(H63)=FVAR(3)
5.a :
 C59'(C60',C61',C62',C63',C64,C65,C66)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C44(H44A,H44B), C51(H51A,H51B),
 C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C107(H10A,H10B), C114(H11A,
 H11B), C127(H12A,H12B), C128(H12C,H12D), C129(H12E,H12F), C130(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41A),
 C42(H42), C43(H43), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C53(H53),
  C54(H54), C55(H55), C56(H56), C57(H57), C59(H59), C60(H60), C61(H61),
 C62(H62), C63(H63), C59'(H59'), C60'(H60'), C61'(H61'), C62'(H62'), C63'(H63'),
  C70(H70), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76), C77(H77),
 C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85), C86(H86),
  C87(H87), C88(H88), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94),
 C96(H96), C97(H97), C98(H98), C99(H99), C100(H100), C102(H102), C103(H103),
 C104(H104), C105(H105), C106(H106), C109(H109), C110(H110), C111(H111),
 C112(H112), C113(H113), C116(H116), C117(H117), C118(H118), C119(H119),
 C120(H120), C122(H122), C123(H123), C124(H124), C125(H125), C126(H126),
 C39A(H39A), C40A(H40A)
;
_shelx_res_checksum              96478
_shelx_hkl_checksum              75965
_olex2_submission_special_instructions 'No special instructions were received'