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_4345434
_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            'C31 H46 N O4 V'
_chemical_formula_weight         547.63
_chemical_name_common            12a
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_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_method           SHELXL-2014/7
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_cell_angle_beta                 91.592(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   30.340(2)
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_cell_measurement_theta_min      2.43
_cell_volume                     3082.7(4)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.974
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_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        23.484
_diffrn_reflns_theta_max         23.484
_diffrn_reflns_theta_min         1.784
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.9572
_exptl_absorpt_correction_T_min  0.8543
_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            dark_brown
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_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.405
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4421
_refine_ls_number_restraints     903
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0945
_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^)+(0.0455P)^2^+17.1733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.2300
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3360
_reflns_number_total             4421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02322_si_002.cif
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_shelx_shelxl_version_number     2014/7
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_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              71564
_shelx_hkl_checksum              61936