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_7123283
_publ_section_title
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 Catalytic hydrazine disproportionation mediated by a thiolate-bridged VFe
 complex
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00345B
_journal_year                    2019
_chemical_formula_moiety         'C59 H61 N P3 S3 Si V, 4(C4 H8 O)'
_chemical_formula_sum            'C75 H93 N O4 P3 S3 Si V'
_chemical_formula_weight         1340.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-07
_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                117.261(2)
_cell_angle_beta                 102.796(2)
_cell_angle_gamma                100.327(2)
_cell_formula_units_Z            2
_cell_length_a                   15.9471(8)
_cell_length_b                   16.4072(8)
_cell_length_c                   16.4690(7)
_cell_measurement_reflns_used    9586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.980
_cell_measurement_theta_min      2.412
_cell_volume                     3534.0(3)
_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      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            115744
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.328
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.7128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0780 before and 0.0584 after correction. The Ratio of minimum to maximum transmission is 0.9551. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         16220
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0670P)^2^+5.0920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12494
_reflns_number_total             16220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00345b2.cif
_cod_data_source_block           compound7
_cod_database_code               7123283
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.931
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C70, C69, C68, O5, C71
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C77, O4, C75, C73, C74, C79, O3, C78, C72
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C70 \\sim C69 \\sim C68 \\sim O5 \\sim C71: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O4 \\sim C75 \\sim C73 \\sim C74 \\sim C76 \\sim C79 \\sim O3 \\sim C78 \\sim
C72 \\sim C77: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(O5) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
4. Others
 Sof(O4)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C76)=
 Sof(H76A)=Sof(H76B)=Sof(C79)=Sof(H79A)=Sof(H79B)=1-FVAR(1)
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(O3)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=
 Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 Si1(H1), C49(H49), C52(H52), C37(H37), C40(H40)
5.b Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C67(H67A,H67B), C64(H64A,H64B), C63(H63A,H63B), C62(H62A,
 H62B), C65(H65A,H65B), C66(H66A,H66B), C61(H61A,H61B), C69(H69A,H69B),
 C68(H68B,H68A), C71(H71A,H71B), C70(H70B,H70A), C75(H75A,H75B), C78(H78A,H78B),
  C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C77(H77A,H77B), C76(H76A,
 H76B), C79(H79A,H79B)
5.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C45(H45), C29(H29), C27(H27), C28(H28), C55(H55), C46(H46),
 C32(H32), C10(H10), C34(H34), C47(H47), C58(H58), C22(H22), C33(H33), C35(H35),
  C3(H3), C57(H57), C5(H5), C59(H59), C56(H56), C24(H24), C2(H2), C1(H1A),
 C23(H23), C12(H12), C11(H11), C17(H17), C4(H4), C13(H13), C16(H16), C15(H15),
 C14(H14)
5.d Fitted pentagon refined as free rotating group:
 C69(C68,O5,C71,C70)
5.e Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C54(H54A,H54B,
 H54C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C38(H38A,
 H38B,H38C)
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_shelx_res_checksum              13966
_olex2_submission_special_instructions 'No special instructions were received'