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_7224916
_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         'C21 H17 Fe N O S5'
_chemical_formula_sum            'C21 H17 Fe N O S5'
_chemical_formula_weight         515.51
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 92.173(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.560(2)
_cell_length_b                   11.0529(14)
_cell_length_c                   20.512(2)
_cell_measurement_reflns_used    7648
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4204.8(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9439
              2theta: -15.0749
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9439
              2theta: -15.0749
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9439
              2theta: -15.0749
;
_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      0.004217
_diffrn_orient_matrix_UB_12      0.049141
_diffrn_orient_matrix_UB_13      -0.021780
_diffrn_orient_matrix_UB_21      -0.090196
_diffrn_orient_matrix_UB_22      0.006308
_diffrn_orient_matrix_UB_23      -0.003232
_diffrn_orient_matrix_UB_31      -0.000070
_diffrn_orient_matrix_UB_32      0.021456
_diffrn_orient_matrix_UB_33      0.043817
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44197
_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    1.228
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2112
_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         0.648
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         7385
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+7.1667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                6341
_reflns_number_total             7385
_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        4204.9(9)
_cod_database_code               7224916
_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 C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C41-S7 = C41-S6
 1.74 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C42 \\sim S6 \\sim S7: within 3.8A with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(S7) = Uanis(S6)
4. Others
 Sof(S6)=Sof(H6a)=Sof(H6b)=Sof(H6c)=1-FVAR(1)
 Sof(S7)=Sof(H42a)=Sof(H42b)=Sof(H42c)=FVAR(1)
5.a Riding coordinates:
 C42(H42a,H42b,H42c), C42(H6a,H6b,H6c)
5.b Secondary CH2 refined with riding coordinates:
 C36(H36a,H36b), C35(H35a,H35b), C14(H14a,H14b), C15(H15a,H15b)
5.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C27(H27), C26(H26), C25(H25), C40(H40), C39(H39), C34(H34),
 C33(H33), C32(H32), C31(H31), C13(H13), C12(H12), C11(H11), C10(H10), C20(H20),
  C18(H18), C4(H4), C5(H5), C6(H6), C7(H7)
5.d Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c)
;
_olex2_submission_special_instructions 'No special instructions were received'