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_7123285
_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         'C41 H29 N P S3 V'
_chemical_formula_sum            'C41 H29 N P S3 V'
_chemical_formula_weight         713.74
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-15 deposited with the CCDC.    2019-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.257(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.1043(11)
_cell_length_b                   17.8047(9)
_cell_length_c                   16.7185(9)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.912
_cell_measurement_theta_min      3.136
_cell_volume                     6848.5(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.98
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0849
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42384
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.605
_diffrn_reflns_theta_min         3.138
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.809
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.5675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0990 before and 0.0792 after correction. The Ratio of minimum to maximum transmission is 0.7525. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       plate
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.789
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6995
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0600P)^2^+21.6430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5007
_reflns_number_total             6995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00345b2.cif
_cod_data_source_block           compound11
_cod_database_code               7123285
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.478
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C38, C39, C40, C41, C42, C43, C36, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18, C19, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24, C25, C26, C27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C36 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C37:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(H38A)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=1-FVAR(1)
 Sof(H38)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=FVAR(1)
 Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C29)=Sof(C24)=Sof(H24)=Sof(C27)=
 Sof(H27)=Sof(C28)=Sof(H28)=1-FVAR(2)
 Sof(C23)=Sof(C22)=Sof(H22)=Sof(C18)=Sof(H18)=Sof(C21)=Sof(H21)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(H20)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C1(H1), C47(H47), C31(H31), C22(H22), C13(H13), C10(H10), C14(H14),
 C6(H6), C18(H18), C2(H2), C33(H33), C7(H7), C46(H46), C3(H3), C45(H45),
 C32(H32), C9(H9), C21(H21), C5(H5), C4(H4), C19(H19), C20(H20), C8(H8),
 C38(H38), C38(H38A), C39(H39), C40(H40), C42(H42), C43(H43), C36(H36),
 C37(H37), C25(H25), C26(H26), C24(H24), C27(H27), C28(H28)
;
_shelx_res_checksum              14297
_olex2_submission_special_instructions 'No special instructions were received'