Catalytic hydrazine disproportionation mediated by a thiolate-bridged VFe complex
Gu, Nina Xiao; Ung, Gaël; Peters, Jonas C.; Chemical Communications  (2019) –; doi:10.1039/C9CC00345B

data_7123284
_publ_section_title
;
 Catalytic hydrazine disproportionation mediated by a thiolate-bridged VFe
 complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00345B
_journal_year                    2019
_chemical_formula_moiety
'C59 H60 Fe N3 P3 S3 Si V, C5 H5 N, 0.96(C4 H10 O)'
_chemical_formula_sum            'C67.82 H74.56 Fe N4 O0.95 P3 S3 Si V'
_chemical_formula_weight         1285.02
_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
_audit_creation_date             2018-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-01-15 deposited with the CCDC.    2019-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.207(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.535(4)
_cell_length_b                   19.966(5)
_cell_length_c                   19.830(5)
_cell_measurement_reflns_used    5759
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      47.67
_cell_measurement_theta_min      2.82
_cell_volume                     6134(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1345
_diffrn_reflns_av_unetI/netI     0.1598
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9165
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        37.496
_diffrn_reflns_theta_max         37.496
_diffrn_reflns_theta_min         2.852
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.422
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1487 before and 0.0833 after correction. The Ratio of minimum to maximum transmission is 0.5881. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       blade
_exptl_crystal_F_000             2693
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.00019(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   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         3042
_refine_ls_number_restraints     1155
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.2620
_refine_ls_R_factor_gt           0.1821
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+659.7053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3402
_refine_ls_wR_factor_ref         0.3944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1663
_reflns_number_total             3042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00345b2.cif
_cod_data_source_block           compound8
_cod_database_code               7123284
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.613
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C6) = Uanis(C5)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(O1)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C66)=Sof(H66A)=Sof(H66B)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C67)=Sof(H67A)=Sof(H67B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C17(H17), C14(H14), C2(H2)
5.b Secondary CH2 refined with riding coordinates:
 C66(H66A,H66B), C67(H67A,H67B)
5.c Aromatic/amide H refined with riding coordinates:
 C52(H52), C47(H47), C56(H56), C40(H40), C57(H57), C22(H22), C27(H27),
 C34(H34), C50(H50), C55(H55), C31(H31), C23(H23), C10(H10), C58(H58), C11(H11),
  C9(H9), C51(H51), C32(H32), C44(H44), C29(H29), C35(H35), C45(H45), C59(H59),
 C8(H8), C39(H39), C28(H28), C43(H43), C33(H33), C46(H46), C62(H62), C60(H60),
 C64(H64), C63(H63), C61(H61), C20(H20), C38(H38), C21(H21)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C13(H13A,H13B,H13C), C6(H6A,H6B,H6C),
 C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C65(H65A,H65B,
 H65C), C1(H1A,H1B,H1C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              1590
_olex2_submission_special_instructions 'No special instructions were received'