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_4345430
_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            'C44 H54 Cl0 N2 O7 V2'
_chemical_formula_weight         824.77
_chemical_name_common            10c
_space_group_crystal_system      monoclinic
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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
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_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   13.5350(8)
_cell_measurement_reflns_used    4172
_cell_measurement_temperature    200(2)
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_cell_measurement_theta_min      2.14
_cell_volume                     4897.2(5)
_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.982
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_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22137
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        22.268
_diffrn_reflns_theta_max         22.268
_diffrn_reflns_theta_min         1.692
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.9540
_exptl_absorpt_correction_T_min  0.8925
_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    1.119
_exptl_crystal_description       hexahedron
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_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         6121
_refine_ls_number_restraints     852
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0617P)^2^+12.8041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4408
_reflns_number_total             6121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02322_si_002.cif
_cod_data_source_block           cos9_sq
_cod_database_code               4345430
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.901
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              76809
_shelx_hkl_checksum              69205
_shelx_fab_checksum              69369