Reactions of dinuclear Ni2 complexes [Ni(RNPyS4)]2 (RNPyS4 = 2,6-bis(2-mercaptophenylthiomethyl-4-R-pyridine) with Fe(CO)3(BDA) (BDA = benzylidene acetone) leading to heterodinuclear NiFe and mononuclear Fe complexes related to the active sites of [NiFe]- and [Fe]-hydrogenases
Song, Li-Cheng; Lu, Yu; Meng, Cao; Yang, Xi-Yue; RSC Adv.  (2016) –; doi:10.1039/C6RA07488J

data_7224915
_publ_section_title
;
 Reactions of dinuclear Ni2 complexes [Ni(RNPyS4)]2 (RNPyS4 =
 2,6-bis(2-mercaptophenylthiomethyl-4-R-pyridine) with Fe(CO)3(BDA) (BDA =
 benzylidene acetone) leading to heterodinuclear NiFe and mononuclear Fe
 complexes related to the active sites of [NiFe]- and [Fe]-hydrogenases
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA07488J
_journal_year                    2016
_chemical_formula_moiety
'C27 H21 Fe N O2 S4, 0.25(C Cl2), 0.25(C H2 Cl2)'
_chemical_formula_sum            'C27.5 H22 Cl Fe N O2 S4'
_chemical_formula_weight         618.00
_chemical_name_systematic
;
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-02 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.107(2)
_cell_angle_beta                 93.721(2)
_cell_angle_gamma                100.053(2)
_cell_formula_units_Z            8
_cell_length_a                   13.4113(10)
_cell_length_b                   14.1978(10)
_cell_length_c                   28.753(2)
_cell_measurement_reflns_used    15503
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     5379.0(7)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9809
              2theta: -15.0892
scan:
    Number of images: 300
               Slice: -105.0000 - 45.0000
         Image width: 0.5000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9809
              2theta: -15.0892
scan:
    Number of images: 200
               Slice: -105.0000 - -5.0000
         Image width: 0.5000
            Exp time: 1.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9809
              2theta: -15.0892
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.048498
_diffrn_orient_matrix_UB_12      0.055289
_diffrn_orient_matrix_UB_13      -0.018731
_diffrn_orient_matrix_UB_21      0.020779
_diffrn_orient_matrix_UB_22      -0.022894
_diffrn_orient_matrix_UB_23      -0.064512
_diffrn_orient_matrix_UB_31      -0.024509
_diffrn_orient_matrix_UB_32      0.019477
_diffrn_orient_matrix_UB_33      -0.015325
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            46111
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2536
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1343
_refine_ls_number_reflns         18489
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                15872
_reflns_number_total             18489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra07488j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        5379.1(7)
_cod_original_formula_sum        'C27.50 H22 Cl Fe N O2 S4'
_cod_database_code               7224915
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C109-Cl1 = C109-Cl2 = C10'-Cl1' = C10'-Cl2'
 1.78 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl1' \\sim Cl2' \\sim C109 \\sim C10': within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl1') \\sim Ueq, Uanis(Cl2')
\\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C10') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(Cl1')=Sof(Cl2')=Sof(C10')=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C109)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C14(H14a,H14b), C22(H22a,H22b), C35(H35a,H35b), C41(H41a,H41b),
 C48(H48a,H48b), C62(H62a,H62b), C68(H68a,H68b), C75(H75a,H75b), C89(H89a,H89b),
  C95(H95a,H95b), C102(H10a,H10b), C110(H11a,H11b)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C16(H16), C17(H17),
 C18(H18), C19(H19), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
  C31(H31), C32(H32), C33(H33), C37(H37), C39(H39), C43(H43), C44(H44),
 C45(H45), C46(H46), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C57(H57),
  C58(H58), C59(H59), C60(H60), C64(H64), C66(H66), C70(H70), C71(H71),
 C72(H72), C73(H73), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C84(H84),
  C85(H85), C86(H86), C87(H87), C91(H91), C93(H93), C97(H97), C98(H98),
 C99(H99), C100(H100), C104(H104), C105(H105), C106(H106), C107(H107),
 C108(H108)
;
_olex2_submission_special_instructions 'No special instructions were received'