Vanadium(V) Complexes with Substituted 1,5-bis(2-hydroxybenzaldehyde)carbohydrazones and Their Use As Catalyst Precursors in Oxidation of Cyclohexane.
Dragancea, Diana; Talmaci, Natalia; Shova, Sergiu; Novitchi, Ghenadie; Darvasiová, Denisa; Rapta, Peter; Breza, Martin; Galanski, Markus; Kož\?íšek, Jozef; Martins, Nuno M. R.; Martins, Luísa M D R S; Pombeiro, Armando J. L.; Arion, Vladimir B.; Inorganic chemistry 55 (2016) 9187–9203; doi:10.1021/acs.inorgchem.6b01011

data_4348137
_publ_section_title
;
 Vanadium(V) Complexes with Substituted
 1,5-bis(2-hydroxybenzaldehyde)carbohydrazones and Their Use As Catalyst
 Precursors in Oxidation of Cyclohexane.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9187
_journal_page_last               9203
_journal_paper_doi               10.1021/acs.inorgchem.6b01011
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C66 H96 N8 O14 V4, 6(C2 H6 O)'
_chemical_formula_sum            'C78 H132 N8 O20 V4'
_chemical_formula_weight         1705.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                66.678(2)
_cell_angle_beta                 88.415(2)
_cell_angle_gamma                87.740(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2721(2)
_cell_length_b                   14.5422(2)
_cell_length_c                   18.1279(3)
_cell_measurement_reflns_used    55895
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      35.40
_cell_measurement_theta_min      2.30
_cell_volume                     2242.65(8)
_computing_cell_refinement       'X-Area 1.76 (Stoe, 2015)'
_computing_data_collection       'X-Area 1.76 (Stoe, 2015)'
_computing_data_reduction        'LANA 1.63.1 (Stoe, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 Pilatus300K
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33916
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         2.655
_exptl_absorpt_coefficient_mu    3.949
_exptl_absorpt_correction_T_max  0.6742
_exptl_absorpt_correction_T_min  0.1771
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
X-Red32,
Version 1.62.2 (release 14-10-2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       prism
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7744
_refine_ls_number_restraints     535
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0546
_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^)+(0.1086P)^2^+0.2226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6821
_reflns_number_total             7744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01011_si_001.cif
_cod_data_source_block           vv2
_cod_database_code               4348137
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H9A of O9, H8 of O8, All C(H,H) groups, All C(H,H,H)
  groups, All N(H) groups
 At 1.5 times of:
  H10X of O10X, H10 of O10
2. Restrained distances
 O10-C38 \\sim O10X-C38X
 with sigma of 0.01
 C39-C38 \\sim C39X-C38X
 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Others
 Sof(O10)=Sof(H10)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=1-FVAR(1)
 Sof(O10X)=Sof(H10X)=Sof(C38X)=Sof(H38C)=Sof(H38D)=Sof(C39X)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=FVAR(1)
6.a Riding coordinates:
 O10(H10), C38(H38A,H38B), C39(H39A,H39B,H39C), O10X(H10X), C38X(H38C,H38D),
 C39X(H39D,H39E,H39F)
6.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C36(H36A,H36B), C34(H34A,H34B)
6.c Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C35(H35A,H35B,
 H35C)
6.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C13(H13)
;
_shelx_res_checksum              78847
_shelx_hkl_checksum              73014
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'