#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:30:02 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239867 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/03/4350391.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4350391
loop_
_publ_author_name
'Zhang, Xian-Ming'
'Hou, Juan-Juan'
'Zhang, Wei-Xiong'
'Chen, Xiao-Ming'
_publ_section_title
;
 Two mixed-valence vanadium(III,IV) phosphonoacetates with 16-ring
 channels: H2(DABCO)[V(IV)O(H2O)V(III)(OH)(O3PCH2CO2)2].2.5H2O and
 H2(PIP)[V(IVO)(H2O)V(III)(OH)(O3PCH2CO2)2].2.5H2O.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8120
_journal_page_last               8125
_journal_paper_doi               10.1021/ic060771p
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C10 H26 N2 O15.5 P2 V2'
_chemical_formula_weight         586.15
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0479(10)
_cell_length_b                   15.307(2)
_cell_length_c                   17.537(3)
_cell_measurement_temperature    298(2)
_cell_volume                     1891.9(5)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Apex CCD Diffractometer'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8086
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  0.9069
_exptl_absorpt_correction_T_min  0.7296
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Sheldrick 1997'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.058
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1852
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0496P)²+9.0605P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1333
_reflns_number_gt                1735
_reflns_number_total             1852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060771psi20060614_113937.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      Pnna
_cod_original_formula_sum        'C10 H26 N2 O15.50 P2 V2'
_cod_database_code               4350391
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
V1 V 0.25449(13) 0.2500 0.2500 0.0166(3) Uani 1 2 d S
V2 V 0.0000 0.0000 0.5000 0.0285(3) Uani 1 2 d S
P1 P 0.25542(13) 0.13521(6) 0.40046(5) 0.0131(3) Uani 1 1 d .
O1 O 0.0274(6) 0.2500 0.2500 0.0292(10) Uani 1 2 d S
O2 O 0.2990(4) 0.14619(17) 0.31612(15) 0.0189(6) Uani 1 1 d .
O3 O 0.4338(4) 0.10747(16) 0.44377(15) 0.0162(6) Uani 1 1 d .
O4 O 0.0902(4) 0.07294(16) 0.41373(14) 0.0147(6) Uani 1 1 d .
O5 O 0.3728(6) 0.3659(2) 0.4575(2) 0.0470(10) Uani 1 1 d .
O6 O 0.3122(5) 0.33010(18) 0.33850(16) 0.0250(7) Uani 1 1 d .
O7 O 0.2500 0.0000 0.5429(2) 0.0153(8) Uani 1 2 d S
H7A H 0.2500 0.0000 0.5960 0.018 Uiso 1 2 calc SR
N1 N 0.1175(7) 0.4479(3) 0.6737(3) 0.0547(14) Uani 1 1 d .
H1A H 0.0171 0.4105 0.6738 0.066 Uiso 1 1 calc R
C1 C 0.2980(6) 0.3170(3) 0.4115(2) 0.0224(9) Uani 1 1 d .
C2 C 0.1819(6) 0.2401(2) 0.4372(2) 0.0209(8) Uani 1 1 d .
H2A H 0.0511 0.2499 0.4223 0.025 Uiso 1 1 calc R
H2B H 0.1855 0.2377 0.4924 0.025 Uiso 1 1 calc R
C3 C 0.2798(10) 0.4050(4) 0.6377(5) 0.065(2) Uani 1 1 d .
H3A H 0.2436 0.3809 0.5887 0.078 Uiso 1 1 calc R
H3B H 0.3262 0.3580 0.6697 0.078 Uiso 1 1 calc R
C4 C 0.0684(13) 0.5262(5) 0.6276(8) 0.141(6) Uani 1 1 d .
H4A H -0.0533 0.5492 0.6438 0.170 Uiso 1 1 calc R
H4B H 0.0588 0.5103 0.5742 0.170 Uiso 1 1 calc R
C5 C 0.156(2) 0.4748(7) 0.7503(5) 0.155(7) Uani 1 1 d .
H5A H 0.1652 0.4241 0.7833 0.186 Uiso 1 1 calc R
H5B H 0.0543 0.5118 0.7689 0.186 Uiso 1 1 calc R
O1W O 0.5819(7) 0.2500 0.2500 0.0394(12) Uani 1 2 d S
H1WA H 0.663(10) 0.231(4) 0.288(3) 0.062(19) Uiso 1 1 d .
O2W O 0.2491(6) 0.8216(3) 0.6255(3) 0.0589(12) Uani 1 1 d D
H2WA H 0.323(8) 0.845(4) 0.593(3) 0.071 Uiso 1 1 d D
H2WB H 0.239(10) 0.857(3) 0.663(2) 0.071 Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 V1 O2 99.06(8) . 4
O1 V1 O2 99.06(9) . .
O2 V1 O2 161.89(17) 4 .
O1 V1 O6 101.62(9) . .
O2 V1 O6 86.06(11) 4 .
O2 V1 O6 90.30(11) . .
O1 V1 O6 101.62(9) . 4
O2 V1 O6 90.30(11) 4 4
O2 V1 O6 86.06(11) . 4
O6 V1 O6 156.76(19) . 4
O1 V1 O1W 180.000(1) . .
O2 V1 O1W 80.94(8) 4 .
O2 V1 O1W 80.94(8) . .
O6 V1 O1W 78.38(9) . .
O6 V1 O1W 78.38(9) 4 .
O7 V2 O7 180.00(19) 5_556 .
O7 V2 O3 88.79(9) 5_556 6_556
O7 V2 O3 91.21(9) . 6_556
O7 V2 O3 91.21(9) 5_556 2
O7 V2 O3 88.79(9) . 2
O3 V2 O3 180.0 6_556 2
O7 V2 O4 89.70(11) 5_556 .
O7 V2 O4 90.30(11) . .
O3 V2 O4 89.29(11) 6_556 .
O3 V2 O4 90.71(11) 2 .
O7 V2 O4 90.30(11) 5_556 5_556
O7 V2 O4 89.70(11) . 5_556
O3 V2 O4 90.71(11) 6_556 5_556
O3 V2 O4 89.29(11) 2 5_556
O4 V2 O4 180.0 . 5_556
O2 P1 O4 111.85(15) . .
O2 P1 O3 110.37(15) . .
O4 P1 O3 112.28(14) . .
O2 P1 C2 107.85(17) . .
O4 P1 C2 106.42(17) . .
O3 P1 C2 107.80(18) . .
P1 O2 V1 128.53(17) . .
P1 O3 V2 132.38(15) . 2
P1 O4 V2 135.51(16) . .
C1 O6 V1 130.4(3) . .
V2 O7 V2 133.72(19) . 2
V2 O7 H7A 113.1 . .
V2 O7 H7A 113.1 2 .
C5 N1 C3 112.7(9) . .
C5 N1 C4 108.9(8) . .
C3 N1 C4 108.0(7) . .
C5 N1 H1A 109.1 . .
C3 N1 H1A 109.1 . .
C4 N1 H1A 109.1 . .
O5 C1 O6 121.6(4) . .
O5 C1 C2 121.1(4) . .
O6 C1 C2 117.2(4) . .
C1 C2 P1 115.7(3) . .
C1 C2 H2A 108.4 . .
P1 C2 H2A 108.4 . .
C1 C2 H2B 108.4 . .
P1 C2 H2B 108.4 . .
H2A C2 H2B 107.4 . .
N1 C3 C4 107.0(5) . 2_565
N1 C3 H3A 110.3 . .
C4 C3 H3A 110.3 2_565 .
N1 C3 H3B 110.3 . .
C4 C3 H3B 110.3 2_565 .
H3A C3 H3B 108.6 . .
N1 C4 C3 109.4(6) . 2_565
N1 C4 H4A 109.8 . .
C3 C4 H4A 109.8 2_565 .
N1 C4 H4B 109.8 . .
C3 C4 H4B 109.8 2_565 .
H4A C4 H4B 108.2 . .
N1 C5 C5 108.0(6) . 2_565
N1 C5 H5A 110.1 . .
C5 C5 H5A 110.1 2_565 .
N1 C5 H5B 110.1 . .
C5 C5 H5B 110.1 2_565 .
H5A C5 H5B 108.4 . .
V1 O1W H1WA 128(4) . .
H2WA O2W H2WB 107.7(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.601(4) .
V1 O2 1.992(3) 4
V1 O2 1.992(3) .
V1 O6 2.019(3) .
V1 O6 2.019(3) 4
V1 O1W 2.307(5) .
V2 O7 1.9161(14) 5_556
V2 O7 1.9161(14) .
V2 O3 1.974(3) 6_556
V2 O3 1.974(3) 2
V2 O4 1.985(2) .
V2 O4 1.985(2) 5_556
P1 O2 1.520(3) .
P1 O4 1.523(3) .
P1 O3 1.529(3) .
P1 C2 1.805(4) .
O3 V2 1.974(3) 2
O5 C1 1.220(5) .
O6 C1 1.299(5) .
O7 V2 1.9161(14) 2
O7 H7A 0.9300 .
N1 C5 1.430(10) .
N1 C3 1.462(8) .
N1 C4 1.487(10) .
N1 H1A 0.9100 .
C1 C2 1.503(6) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.511(9) 2_565
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C3 1.511(9) 2_565
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C5 1.53(2) 2_565
C5 H5A 0.9700 .
C5 H5B 0.9700 .
O1W H1WA 0.93(6) .
O2W H2WA 0.859(10) .
O2W H2WB 0.860(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O6 0.91 1.91 2.816(5) 173.3 6_556
O1W H1WA O2W 0.93(6) 1.83(6) 2.719(5) 161(6) 5_666
O2W H2WA O3 0.859(10) 1.97(3) 2.766(5) 154(7) 5_666
