#------------------------------------------------------------------------------
#$Date: 2018-06-14 06:45:12 +0300 (Thu, 14 Jun 2018) $
#$Revision: 208362 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/00/2010048.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2010048
loop_
_publ_author_name
'Neves, Ademir'
'Vencato, Ivo'
'Mascarenhas, Yvonne P.'
_publ_contact_author
;
    Dr Ivo Vencato
    Depto. Física - UFSC
    88040 - 900 Florianópolis, SC
    Brazil
;
_publ_section_title
;[N,N'-Bis(2-hydroxybenzyl)-N-methyl-N'-(2-pyridylmethyl)-1,3-propanediamine]oxovanadium(IV)
 hemihydrate, [VO(bbmppn)].0.5H₂O
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1417
_journal_page_last               1419
_journal_paper_doi               10.1107/S0108270194002672
_journal_volume                  50
_journal_year                    1994
_chemical_formula_analytical     'VO(C~24~ H~27~ N~3~ O~2~),0.5H~2~O'
_chemical_formula_sum            'C24 H28 N3 O3.5 V'
_chemical_formula_weight         465.4
_chemical_name_systematic
;
 oxo (N,N'-bis(2-hydroxybenzyl)-N-(methyl)-N'-
(pyridylmethyl) -1,3-propanodiamine)-vanadium (IV) hemihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_type_scat_source
;
 International Tables for X-ray Crystallography (1974, Vol.IV)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.03(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.520(3)
_cell_length_b                   6.840(2)
_cell_length_c                   18.241(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      17.2
_cell_volume                     4332.8(15)
_computing_cell_refinement       'SDP-Plus (Frenz, 1985)'
_computing_data_collection       'SDP-Plus (Frenz, 1985)'
_computing_data_reduction        'SDP-Plus (Frenz, 1985)'
_computing_molecular_graphics    'ORTEP (Johnson, 1975)'
_computing_structure_refinement  'SHELX76 (Sheldrick, 1976)'
_computing_structure_solution    'SHELX86 (Sheldrick, 1986)'
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.098
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3632
_diffrn_reflns_theta_max         60.1
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time  30
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.0
_exptl_absorpt_correction_T_max  1.604
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   'empirical (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.53
_refine_ls_extinction_coef       '\c = 7.4(3) x 10^-8^'
_refine_ls_extinction_method     'F =  F(1-\cF²/sinθ)'
_refine_ls_goodness_of_fit_obs   5.09
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         2153
_refine_ls_R_factor_obs          0.0747
_refine_ls_shift/esd_max         0.09
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 5.834/[σ²(F) + 0.000818F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0823
_reflns_number_observed          2153
_reflns_number_total             2825
_reflns_observed_criterion       F>6.0\s(F)
_cod_data_source_file            li1102.cif
_cod_data_source_block           default
_cod_depositor_comments
;
 Updating space group information and adding the symmetry operation list.

 Antanas Vaitkus,
 2018-06-14

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value ' w = 5.834/[\s^2^(F) +
0.000818F^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 5.834/[\s^2^(F) + 0.000818F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4333(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C24 H28 N3 O3.5 V1'
_cod_database_code               2010048
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z+1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
V 0.3962 0.1801(2) 0.60190(10)
O(1) 0.43050(10) 0.2751(7) 0.6698(2)
O(2) 0.37980(10) 0.3678(7) 0.5212(2)
O(3) 0.35230(10) 0.2642(6) 0.6312(2)
N(1) 0.35190(10) -0.0222(8) 0.5247(3)
N(2) 0.4002(2) -0.0938(8) 0.6676(3)
N(3) 0.4393(2) 0.0833(8) 0.5469(3)
C(1) 0.3920(2) 0.4220(10) 0.4627(3)
C(2) 0.3669(2) 0.5220(10) 0.4007(4)
C(3) 0.3795(3) 0.5840(10) 0.3406(4)
C(4) 0.4160(3) 0.5440(10) 0.3396(5)
C(5) 0.4401(3) 0.4420(10) 0.3993(4)
C(6) 0.4293(2) 0.3760(10) 0.4608(4)
C(7) 0.4561(2) 0.2660(10) 0.5257(4)
C(8) 0.4246(2) -0.0390(10) 0.4768(4)
C(9) 0.4719(2) -0.0160(10) 0.6036(4)
C(10) 0.4620(2) -0.1970(10) 0.6421(4)
C(11) 0.4409(2) -0.1600(10) 0.7001(4)
C(12) 0.3860(2) -0.0430(10) 0.7334(3)
C(13) 0.3439(2) 0.0010(10) 0.7095(3)
C(14) 0.3188(3) -0.1110(10) 0.7376(4)
C(15) 0.2806(2) -0.0630(10) 0.7177(4)
C(16) 0.2666(2) 0.0890(10) 0.6693(4)
C(17) 0.2905(2) 0.2010(10) 0.6399(4)
C(18) 0.3298(2) 0.1527(9) 0.6601(3)
C(19) 0.3772(2) -0.2610(10) 0.6242(3)
C(20) 0.3457(2) -0.1920(10) 0.5566(4)
C(21) 0.3132(2) -0.3080(10) 0.5258(4)
C(22) 0.2858(2) -0.2410(10) 0.4608(4)
C(23) 0.2922(2) -0.0690(10) 0.4270(4)
C(24) 0.3247(2) 0.0350(10) 0.4613(4)
O(W) 0.5000 0.4420(10) 0.7500
H(W) 0.4759 0.3638 0.7258
H(2) 0.3380 0.5591 0.4033
H(3) 0.3589 0.6736 0.2924
H(4) 0.4244 0.5938 0.2905
H(5) 0.4708 0.4059 0.3991
H(7') 0.4667 0.3552 0.5758
H(7") 0.4811 0.2181 0.5077
H(8) 0.4009 0.0249 0.4345
H(8') 0.4150 -0.1822 0.4942
H(8") 0.4474 -0.0739 0.4520
H(9') 0.4923 -0.0603 0.5728
H(9") 0.4862 0.0822 0.6488
H(10') 0.4446 -0.2922 0.5950
H(10") 0.4891 -0.2763 0.6686
H(11') 0.4567 -0.0547 0.7415
H(11") 0.4403 -0.2986 0.7311
H(12') 0.4017 0.0807 0.7649
H(12") 0.3914 -0.1686 0.7734
H(14) 0.3306 -0.2429 0.7751
H(15) 0.2609 -0.1495 0.7387
H(16) 0.2361 0.1273 0.6547
H(17) 0.2799 0.3255 0.6019
H(19') 0.3963 -0.3595 0.6047
H(19") 0.3656 -0.3458 0.6625
H(21) 0.3112 -0.4546 0.5525
H(22) 0.2587 -0.3202 0.4366
H(23) 0.2716 -0.0225 0.3734
H(24) 0.3289 0.1776 0.4367
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(1) V O(2) 107.9(2) yes
O(1) V O(3) 100.5(2) yes
O(1) V N(1) 165.5(2) yes
O(1) V N(2) 91.1(2) yes
O(1) V N(3) 88.6(2) yes
O(2) V O(3) 85.6(2) yes
O(2) V N(1) 86.4(2) yes
O(2) V N(2) 160.9(2) yes
O(2) V N(3) 87.1(2) yes
O(3) V N(1) 81.9(2) yes
O(3) V N(2) 91.4(2) yes
O(3) V N(3) 169.7(2) yes
N(1) V N(2) 74.5(2) yes
N(1) V N(3) 90.4(2) yes
N(2) V N(3) 93.2(2) yes
C(20) N(1) C(24) 116.7(6) no
C(11) N(2) C(12) 107.7(5) no
C(11) N(2) C(19) 107.8(5) no
C(12) N(2) C(19) 109.1(5) no
C(7) N(3) C(8) 108.5(5) no
C(7) N(3) C(9) 105.0(5) no
C(8) N(3) C(9) 110.0(5) no
O(2) C(1) C(2) 119.2(6) no
O(2) C(1) C(6) 121.6(6) no
C(2) C(1) C(6) 119.2(7) no
C(1) C(2) C(3) 119.8(7) no
C(2) C(3) C(4) 121.0(8) no
C(3) C(4) C(5) 118.9(9) no
C(4) C(5) C(6) 122.9(8) no
C(1) C(6) C(5) 118.1(7) no
C(1) C(6) C(7) 119.8(6) no
C(5) C(6) C(7) 122.1(7) no
N(3) C(7) C(6) 114.0(6) no
N(3) C(9) C(10) 116.2(6) no
C(9) C(10) C(11) 115.6(6) no
N(2) C(11) C(10) 115.8(6) no
N(2) C(12) C(13) 113.3(6) no
C(12) C(13) C(14) 120.8(6) no
C(12) C(13) C(18) 119.3(6) no
C(14) C(13) C(18) 119.9(6) no
C(13) C(14) C(15) 119.9(7) no
C(14) C(15) C(16) 120.3(8) no
C(15) C(16) C(17) 121.3(8) no
C(16) C(17) C(18) 118.8(7) no
O(3) C(18) C(13) 122.6(6) no
O(3) C(18) C(17) 117.6(6) no
C(13) C(18) C(17) 119.8(6) no
N(2) C(19) C(20) 111.2(5) no
N(1) C(20) C(19) 116.3(6) no
N(1) C(20) C(21) 123.5(6) no
C(19) C(20) C(21) 120.0(6) no
C(20) C(21) C(22) 117.4(7) no
C(21) C(22) C(23) 119.4(8) no
C(22) C(23) C(24) 119.0(7) no
N(1) C(24) C(23) 123.9(7) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
V O(1) 1.602(5) yes
V O(2) 1.905(5) yes
V O(3) 1.928(5) yes
V N(1) 2.259(5) yes
V N(2) 2.204(5) yes
V N(3) 2.214(6) yes
O(2) C(1) 1.330(8) no
O(3) C(18) 1.343(8) no
N(1) C(20) 1.349(8) no
N(1) C(24) 1.329(8) no
N(2) C(11) 1.490(9) no
N(2) C(12) 1.488(8) no
N(2) C(19) 1.493(8) no
N(3) C(7) 1.495(9) no
N(3) C(8) 1.483(8) no
N(3) C(9) 1.479(9) no
C(1) C(2) 1.390(10) no
C(1) C(6) 1.410(10) no
C(2) C(3) 1.380(10) no
C(3) C(4) 1.37(2) no
C(4) C(5) 1.360(10) no
C(5) C(6) 1.380(10) no
C(6) C(7) 1.490(10) no
C(9) C(10) 1.520(10) no
C(10) C(11) 1.510(10) no
C(12) C(13) 1.490(10) no
C(13) C(14) 1.410(10) no
C(13) C(18) 1.366(9) no
C(14) C(15) 1.370(10) no
C(15) C(16) 1.360(10) no
C(16) C(17) 1.390(10) no
C(17) C(18) 1.410(10) no
C(19) C(20) 1.479(9) no
C(20) C(21) 1.390(10) no
C(21) C(22) 1.370(10) no
C(22) C(23) 1.380(10) no
C(23) C(24) 1.360(10) no
