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_7043632
_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_formula_moiety         'C28 H27 Br2 N Ni O2 P2, 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C29 H29 Br2 Cl2 N Ni O2 P2'
_chemical_formula_weight         774.90
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.729(3)
_cell_length_b                   17.2262(18)
_cell_length_c                   8.1747(12)
_cell_measurement_reflns_used    8490
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.1
_cell_volume                     3200.7(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 0.993
_diffrn_measurement_device_type  'Rigaku Saturn 724CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            28192
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.937
_diffrn_reflns_theta_min         2.147
_exptl_absorpt_coefficient_mu    3.397
_exptl_absorpt_correction_T_max  0.6860
_exptl_absorpt_correction_T_min  0.5498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3940
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0556P)^2^+3.0094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3630
_reflns_number_total             3940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02203d2.cif
_cod_data_source_block           m130306b1
_cod_database_code               7043632
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.686
_shelx_estimated_absorpt_t_min   0.550
_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
 Cl1-C17 = Cl2-C17 = Cl1'-C17' = Cl2'-C17'
 1.72 with sigma of 0.01
 Cl1-Cl2 = Cl1'-Cl2'
 2.8 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C17')
4. Others
 Sof(Cl1')=Sof(Cl2')=Sof(C17')=Sof(H17C)=Sof(H17D)=0.5*(1-FVAR(2))
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(Cl1)=Sof(Cl2)=0.5*FVAR(2)
 Fixed Sof: H13A(0.5) H13B(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5)
5.a Riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B,H16C), C17(H17A,H17B), C17'(H17C,H17D)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B)
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)
;
_shelx_res_checksum              1088
_olex2_submission_special_instructions 'No special instructions were received'