Vanadium complexes with multidentate amine bisphenols.
Hänninen, M M; Peuronen, A.; Damlin, P.; Tyystjärvi, V; Kivelä, H; Lehtonen, A.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14022–14028; doi:10.1039/c4dt01007h

data_7031854
_publ_section_title
;
 Vanadium complexes with multidentate amine bisphenols.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14022
_journal_page_last               14028
_journal_paper_doi               10.1039/c4dt01007h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C34 H52 N O5 V'
_chemical_formula_sum            'C34 H52 N O5 V'
_chemical_formula_weight         605.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.008(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8297(3)
_cell_length_b                   10.4967(4)
_cell_length_c                   29.3356(10)
_cell_measurement_reflns_used    4536
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      76.2520
_cell_measurement_theta_min      4.5090
_cell_volume                     3330.16(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector_area_resol_mean 5.1977
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0740087000
_diffrn_orient_matrix_UB_12      -0.0085825000
_diffrn_orient_matrix_UB_13      0.0462284000
_diffrn_orient_matrix_UB_21      -0.1181402000
_diffrn_orient_matrix_UB_22      0.0298656000
_diffrn_orient_matrix_UB_23      0.0249646000
_diffrn_orient_matrix_UB_31      -0.0290190000
_diffrn_orient_matrix_UB_32      -0.1434692000
_diffrn_orient_matrix_UB_33      0.0025261000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11251
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.979
_diffrn_reflns_theta_min         3.017
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.2103
_exptl_crystal_size_mid          0.1124
_exptl_crystal_size_min          0.0297
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6451
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0933P)^2^+12.7536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5588
_reflns_number_total             6451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01007h2.cif
_cod_data_source_block           3_vt-1
_cod_depositor_comments
'Adding full bibliography for 7031852--7031855.cif.'
_cod_database_code               7031854
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C32 H51 N1 O5 V1'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34B-C32 = C34A-C32 = C35B-C32 = C35A-C32
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35B \\sim C35A: within 1.7A with sigma of 0.003 and sigma for terminal atoms
of 0.01
Uanis(C34B) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C35B) \\sim Ueq,
Uanis(C35A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.006
4. Others
 Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35B)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=1-FVAR(1)
 Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C19(H19A,H19B), C18(H18A,H18B), C17(H17A,H17B),
 C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C11(H11), C13(H13)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C33(H33A,H33B,H33C),
 C34A(H34A,H34B,H34C), C34B(H34D,H34E,H34F), C35A(H35A,H35B,H35C), C35B(H35D,
 H35E,H35F), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;