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_7123286
_publ_section_title
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 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         'C40 H32 O P S3 V, 0.5(C4 H8 O)'
_chemical_formula_sum            'C42 H36 O1.5 P S3 V'
_chemical_formula_weight         742.80
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-01-15 deposited with the CCDC.    2019-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.749(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.9914(4)
_cell_length_b                   28.6309(12)
_cell_length_c                   27.7030(11)
_cell_measurement_reflns_used    9478
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.453
_cell_measurement_theta_min      3.213
_cell_volume                     7082.2(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.04
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0918
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            307714
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.575
_diffrn_reflns_theta_min         3.087
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.693
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1092 before and 0.0887 after correction. The Ratio of minimum to maximum transmission is 0.7241. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         14478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0490P)^2^+6.5320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12810
_reflns_number_total             14478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00345b2.cif
_cod_data_source_block           PS3VTHF
_cod_original_formula_sum        'C42 H36 O1.50 P S3 V'
_cod_database_code               7123286
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.414
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C79(H79A,H79B), C74(H74A,H74B), C78(H78A,H78B), C73(H73A,H73B), C75(H75A,
 H75B), C77(H77A,H77B), C80(H80A,H80B), C76(H76A,H76B), C81(H81A,H81B),
 C83(H83A,H83B), C84(H84A,H84B), C82(H82A,H82B)
2.b Aromatic/amide H refined with riding coordinates:
 C60(H60), C46(H46), C23(H23), C34(H34), C35(H35), C26(H26), C10(H10), C8(H8),
 C36(H36), C47(H47), C22(H22), C59(H59), C24(H24), C25(H25), C70(H70), C48(H48),
  C49(H49), C29(H29), C61(H61), C9(H9), C65(H65), C72(H72), C27(H27), C58(H58),
 C28(H28), C64(H64), C53(H53), C62(H62), C63(H63), C37(H37), C1(H1), C71(H71),
 C50(H50), C3(H3), C38(H38), C51(H51), C52(H52), C2(H2), C4(H4), C5(H5),
 C41(H41), C13(H13), C17(H17), C39(H39), C40(H40), C16(H16), C15(H15), C14(H14)
;
_shelx_res_checksum              19712
_olex2_submission_special_instructions 'No special instructions were received'