Synthesis of Mono- and Dinuclear Vanadium Complexes and Their Reactivity toward Dehydroperoxidation of Alkyl Hydroperoxides.
Schmidt, Anna-Corina; Hermsen, Marko; Rominger, Frank; Dehn, Richard; Teles, Joaquim Henrique; Schäfer, Ansgar; Trapp, Oliver; Schaub, Thomas; Inorganic chemistry 56 (2017) 1319–1332; doi:10.1021/acs.inorgchem.6b02322

data_4345431
_publ_section_title
;
 Synthesis of Mono- and Dinuclear Vanadium Complexes and Their Reactivity
 toward Dehydroperoxidation of Alkyl Hydroperoxides.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1319
_journal_page_last               1332
_journal_paper_doi               10.1021/acs.inorgchem.6b02322
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C50 H60 N2 O7 V2'
_chemical_formula_weight         902.88
_chemical_name_common            10c
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
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_cell_angle_gamma                117.7866(19)
_cell_formula_units_Z            2
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_cell_length_c                   15.0994(10)
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_cell_measurement_temperature    200(2)
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_cell_measurement_theta_min      2.42
_cell_volume                     2332.1(3)
_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
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_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18364
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        21.724
_diffrn_reflns_theta_max         21.724
_diffrn_reflns_theta_min         1.432
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.9565
_exptl_absorpt_correction_T_min  0.8769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       long
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_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         5515
_refine_ls_number_restraints     2152
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1052P)^2^+4.7006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2210
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3656
_reflns_number_total             5515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02322_si_002.cif
_cod_data_source_block           cos12
_cod_database_code               4345431
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              24729
_shelx_hkl_checksum              81592