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_4087135
_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         'C36 H31 Fe Ni O3 P2 Se2, C H Cl3, B F4'
_chemical_formula_sum            'C37 H32 B Cl3 F4 Fe Ni O3 P2 Se2'
_chemical_formula_weight         1052.20
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.29(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.860(6)
_cell_length_b                   10.717(2)
_cell_length_c                   26.157(5)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    293.1500
_cell_measurement_theta_max      27.9383
_cell_measurement_theta_min      2.8339
_cell_volume                     8370(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      293.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -110.0000 - 70.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.0317
              2theta: -19.9048
scan:
    Number of images: 150
               Slice: -110.0000 - 40.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.0317
              2theta: -19.9048
scan:
    Number of images: 100
               Slice: -110.0000 - -10.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.0317
              2theta: -19.9048
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0253
_diffrn_orient_matrix_UB_12      -0.0108
_diffrn_orient_matrix_UB_13      -0.0191
_diffrn_orient_matrix_UB_21      0.0607
_diffrn_orient_matrix_UB_22      -0.0266
_diffrn_orient_matrix_UB_23      -0.0657
_diffrn_orient_matrix_UB_31      0.0023
_diffrn_orient_matrix_UB_32      -0.0346
_diffrn_orient_matrix_UB_33      0.0162
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            40118
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.890
_diffrn_reflns_theta_min         2.793
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.00076(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9953
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0667P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7169
_reflns_number_total             9953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00942_si_002.cif
_cod_data_source_block           3b
_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               4087135
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.599
_diffrn_number_total             10475
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C40-Cl1 = C40-Cl2 = C40-Cl3
 1.78 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl3: 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(Cl3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C40(H40)
;
_shelx_res_checksum              43167
_shelx_hkl_checksum              53704
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'