Dithiolato- and halogenido-bridged nickel-iron complexes related to the active site of [NiFe]-H2ases: preparation, structures, and electrocatalytic H2 production
Song, Li-Cheng; Han, Xiao-Feng; Chen, Wei; Li, Jia-Peng; Wang, Xu-Yong; Dalton Trans.  (2017) –; doi:10.1039/C7DT02203D

data_7043633
_publ_section_title
;
 Dithiolato- and halogenido-bridged nickel-iron complexes related to the
 active site of [NiFe]-H2ases: preparation, structures, and
 electrocatalytic H2 production
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02203D
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H29 Br2 N Ni P2, C H2 Cl2'
_chemical_formula_sum            'C33 H31 Br2 Cl2 N Ni P2'
_chemical_formula_weight         792.96
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-06 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.789(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.679(3)
_cell_length_b                   8.898(2)
_cell_length_c                   16.062(4)
_cell_measurement_reflns_used    5711
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.3
_cell_volume                     1668.3(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_detector_area_resol_mean 14.22
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14193
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         1.268
_exptl_absorpt_coefficient_mu    3.256
_exptl_absorpt_correction_T_max  0.6960
_exptl_absorpt_correction_T_min  0.5620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 1102 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0401
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                3889
_reflns_number_total             5868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02203d2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1668.5(8)
_cod_database_code               7043633
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.562
_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
2. Restrained distances
 C33-Cl1 = C33-Cl2 = C33'-Cl1' = C33'-Cl2'
 1.78 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C33')
\\sim Ueq, Uanis(Cl1') \\sim Ueq, Uanis(Cl2') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Cl2) = Uanis(Cl2')
Uanis(Cl1) = Uanis(Cl1')
4. Others
 Sof(Cl1')=Sof(Cl2')=Sof(C33')=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C33)=Sof(H33A)=Sof(H33B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C33(H33A,H33B), C33'(H33C,H33D)
5.b Me refined with riding coordinates:
 C20(H20A,H20B,H20C)
5.c 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), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
;
_shelx_res_checksum              14985
_olex2_submission_special_instructions 'No special instructions were received'