Dithiolato- and Diselenolato-Bridged Nickel‒Iron Biomimetics for the Active Site of [NiFe]Hydrogenases
Song, Li-Cheng; Lu, Yu; Zhu, Liang; Li, Qian-Li; Organometallics 36 (2017) 750–; doi:10.1021/acs.organomet.6b00942

data_4087133
_publ_section_title
;
 Dithiolato- and Diselenolato-Bridged Nickel--Iron Biomimetics for the
 Active Site of [NiFe]Hydrogenases
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              750
_journal_paper_doi               10.1021/acs.organomet.6b00942
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         '2(C36 H30 Fe Ni O3 P2 Se2), 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C73 H62 Cl2 Fe2 Ni2 O6 P4 Se4'
_chemical_formula_weight         1774.96
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.928(8)
_cell_length_b                   11.157(3)
_cell_length_c                   18.479(4)
_cell_measurement_reflns_used    17643
_cell_measurement_temperature    113
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      1.6
_cell_volume                     6995(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)
;
_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                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -120.0000 - 60.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 60.2407
              2theta: -29.9145
scan:
    Number of images: 150
               Slice: -120.0000 - 30.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 60.2407
              2theta: -29.9145
scan:
    Number of images: 100
               Slice: -120.0000 - -20.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 60.2407
              2theta: -29.9145
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.008336
_diffrn_orient_matrix_UB_12      -0.037075
_diffrn_orient_matrix_UB_13      0.038526
_diffrn_orient_matrix_UB_21      -0.085579
_diffrn_orient_matrix_UB_22      -0.025868
_diffrn_orient_matrix_UB_23      -0.006377
_diffrn_orient_matrix_UB_31      0.007487
_diffrn_orient_matrix_UB_32      -0.019685
_diffrn_orient_matrix_UB_33      -0.020619
_diffrn_radiation_monochromator  Multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            53582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.939
_diffrn_reflns_theta_min         1.921
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.238
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8375
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7221
_reflns_number_total             8375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00942_si_002.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/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 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4087133
_shelx_estimated_absorpt_t_max   0.738
_shelx_estimated_absorpt_t_min   0.564
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H6A,H6B} of C6, {H5A,H5B} of C5, {H4A,H4B} of C4
 At 1.5 times of:
  {H37A,H37B} of C37
2. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C37: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Cl2(0.5) C37(0.5) H37A(0.5) H37B(0.5)
4.a Riding coordinates:
 C37(H37A,H37B)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18)
;
_shelx_res_checksum              71308
_shelx_hkl_checksum              86915
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'