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_4087136
_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 H30 D Fe Ni O3 P2 S2, B F4, C H2 Cl2'
_chemical_formula_sum            'C37 H32 B Cl2 D F4 Fe Ni O3 P2 S2'
_chemical_formula_weight         924.97
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.590(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1372(3)
_cell_length_b                   10.1875(2)
_cell_length_c                   24.8639(6)
_cell_measurement_reflns_used    5545
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8640
_cell_measurement_theta_min      4.5510
_cell_volume                     3834.06(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     27.00  70.00   1.00    9.93    --   41.49 -57.00-150.00   43
  2  \w     35.00 136.00   1.00   39.70    --  107.08 -61.00-150.00  101
  3  \w    117.00 171.00   1.00   39.70    --  107.08  15.00  90.00   54
  4  \w     97.00 165.00   1.00   39.70    --  107.08 125.00 -30.00   68
  5  \w     87.00 163.00   1.00   39.70    --  107.08  45.00 150.00   76
  6  \w     68.00 109.00   1.00   39.70    --  107.08 -95.00 120.00   41
  7  \w     43.00 116.00   1.00   39.70    --  107.08-125.00  90.00   73
  8  \w     35.00  61.00   1.00   39.70    --  107.08 -95.00 120.00   26
  9  \w     54.00  80.00   1.00   39.70    --  107.08  15.00  90.00   26
 10  \w    -65.00  -3.00   1.00    9.93    --  -41.49 125.00-180.00   62
 11  \w    -95.00 -66.00   1.00    9.93    --  -41.49 125.00-120.00   29
 12  \w   -108.00 -19.00   1.00    9.93    --  -41.49 -38.00  30.00   89
 13  \w   -114.00 -89.00   1.00    9.93    --  -41.49-142.00 -97.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0514402000
_diffrn_orient_matrix_UB_12      0.0545103000
_diffrn_orient_matrix_UB_13      -0.0488965000
_diffrn_orient_matrix_UB_21      -0.0242789000
_diffrn_orient_matrix_UB_22      -0.1410006000
_diffrn_orient_matrix_UB_23      -0.0171742000
_diffrn_orient_matrix_UB_31      -0.0842690000
_diffrn_orient_matrix_UB_32      0.0072080000
_diffrn_orient_matrix_UB_33      0.0339950000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15143
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         3.56
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         6838
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0846P)^2^+3.8213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                5535
_reflns_number_total             6838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00942_si_002.cif
_cod_data_source_block           4a
_cod_original_cell_volume        3834.07(15)
_cod_database_code               4087136
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F2-B1 \\sim B1-F2'
 with sigma of 0.02
 F1'-B1 \\sim B1-F1
 with sigma of 0.02
 F3'-B1 \\sim B1-F3
 with sigma of 0.02
 F1'-F3' \\sim F3'-F2'
 with sigma of 0.02
 F3'-F2' \\sim F2'-F1'
 with sigma of 0.02
 F3'-F1' \\sim F1'-F2'
 with sigma of 0.02
 F1-F3 \\sim F3-F2
 with sigma of 0.02
 F2-F1 \\sim F1-F3
 with sigma of 0.02
 F2-F3 \\sim F3-F1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1') \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(F2) = Uanis(F2')
Uanis(F1') = Uanis(F1)
Uanis(F3') = Uanis(F3)
4. Others
 Sof(F1')=Sof(F3')=Sof(F2')=1-FVAR(1)
 Sof(F3)=Sof(F2)=Sof(F1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C37(H37A,H37B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
;
_olex2_date_sample_data_collection 2016-09-26
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.783
_oxdiff_exptl_absorpt_empirical_full_min 0.467