A mononuclear oxovanadium(IV) complex [VO(H~2~<i>L</i>)(SO~4~)].5H~2~O derived from a potentially dinucleating tetraaminodiphenol macrocyclic ligand (H~2~<i>L</i>)
Soma Ghosh; Monika Mukherjee; Alok K. Mukherjee; Sasankasekhar Mohanta; Madeleine Helliwell; Acta Crystallographica Section C 50 (1994) 1204–1207; doi:10.1107/S0108270194002209

data_2009975
_publ_section_title
;
 A mononuclear oxovanadium(IV) complex [VO(H~2~<i>L</i>)(SO~4~)].5H~2~O
 derived from a potentially dinucleating tetraaminodiphenol macrocyclic
 ligand (H~2~<i>L</i>)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1204
_journal_page_last               1207
_journal_paper_doi               10.1107/S0108270194002209
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C23 H44 N4 O12 S V'
_chemical_formula_sum            'C23 H44 N4 O12 S V'
_chemical_formula_weight         651.62
_chemical_name_systematic
;(1,5,13,17-tetraamino-9,21-dimethylicosatri-7,9,11,19,21,23-hexen-24,25-diol-
\k^2^N,\k^2^O)oxo(sulfato)vanadium(IV)
 pentahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.46(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.180(10)
_cell_length_b                   12.160(10)
_cell_length_c                   20.580(10)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2987(4)
_computing_cell_refinement       'AFC-5R software'
_computing_data_collection       'AFC-5R software'
_computing_data_reduction        'AFC-5R software'
_computing_molecular_graphics
; ORTEPII (Johnson, 1976); PLUTO NRCVAX (Gabe, Le Page, Charland, Lee &
 White, 1989)
;
_computing_publication_material
;SHELXL93 (Sheldrick, 1993); software for geometric calculations: PARST
(Nardelli, 1983)
;
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELX76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'AFC5R diffractometer'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4689
_diffrn_reflns_theta_max         60.21
_diffrn_reflns_theta_min         3.70
_diffrn_standards_decay_%        4.6
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.004
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.45
_exptl_crystal_density_meas      1.46
_exptl_crystal_density_method    'flotation in?'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.784
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.114
_refine_ls_goodness_of_fit_obs   1.050
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         4396
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.194
_refine_ls_restrained_S_obs      1.046
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_obs          0.0705
_refine_ls_shift/esd_max         -0.165
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w=1/[\s^2^(Fo^2^) + (0.0291P)^2^ + 18.2674P]
 where P=(Fo^2^ + 2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.2094
_refine_ls_wR_factor_obs         0.1487
_reflns_number_observed          3018
_reflns_number_total             4451
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            li1097.cif
_cod_data_source_block           van
_cod_original_cell_volume        2987.(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2009975