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_4345432
_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            'C52 H70 N2 O7 V2'
_chemical_formula_weight         936.98
_chemical_name_common            11c
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6497(11)
_cell_length_b                   11.9057(9)
_cell_length_c                   26.558(2)
_cell_measurement_reflns_used    11678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.33
_cell_measurement_theta_min      3.33
_cell_volume                     4948.3(6)
_computing_cell_refinement       'STOE X-AREA'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'STOE Stadivari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_av_unetI/netI     0.1071
_diffrn_reflns_Laue_measured_fraction_full 0.916
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
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_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        56.910
_diffrn_reflns_theta_max         56.910
_diffrn_reflns_theta_min         3.328
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    3.572
_exptl_absorpt_correction_T_max  1.466
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.830
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3050
_refine_ls_number_restraints     527
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1690
_refine_ls_R_factor_gt           0.1126
_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^)+(0.0631P)^2^+98.3565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2641
_refine_ls_wR_factor_ref         0.2898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1946
_reflns_number_total             3050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02322_si_002.cif
_cod_data_source_block           cos11
_cod_original_cell_volume        4948.4(7)
_cod_database_code               4345432
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.695
_shelx_estimated_absorpt_t_max   0.965
_exptl_absorpt_special_details   'STOE X-AREA Laue Analyzer'
_shelx_res_checksum              13904
_shelx_hkl_checksum              86478