#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006095.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_2006095
loop_
_publ_author_name
'Lees, A. M. J.'
'Platt, A. W. G.'
'Kresin{\`}ski, R. A.'
_publ_section_title
;
Bis[1-hydroxyethane-1,1-diylbis(dimethyl
phosphonate-O)]tris(nitrato-O,O')praseodymium
;
_journal_issue 5
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 581
_journal_page_last 583
_journal_volume 53
_journal_year 1997
_chemical_formula_iupac '[Pr (N1 O3)3 (C6 H16 O7 P2)2]'
_chemical_formula_sum 'C12 H32 N3 O23 P4 Pr'
_chemical_formula_weight 851.20
_chemical_name_common
;
Bis(1,1-bis(dimethylphosphonate)-1-hydroxyethane) praseodymium trinitrate
;
_chemical_name_systematic
;
Bis(1,1-bis(dimethylphosphonato)-1-hydroxyethane) praseodymium (III) nitrate
;
_chemical_temperature_decomposition 160
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_cell_angle_alpha 90
_cell_angle_beta 92.23(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 20.860(4)
_cell_length_b 9.090(2)
_cell_length_c 17.202(3)
_cell_measurement_reflns_used 250
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 25.0
_cell_measurement_theta_min 2.4
_cell_volume 3259.3(11)
_computing_cell_refinement MADNES
_computing_data_collection 'MADNES (Pflugrath & Messerschmidt, 1990)'
_computing_data_reduction MADNES
_computing_molecular_graphics 'SNOOPI (Davies, 1983)'
_computing_publication_material SHELXL93
_computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution 'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measurement_device 'Delft Instruments FAST TV'
_diffrn_measurement_method 'area detector'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0474
_diffrn_reflns_av_sigmaI/netI 0.0942
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 6437
_diffrn_reflns_theta_max 25.02
_diffrn_reflns_theta_min 2.44
_exptl_absorpt_coefficient_mu 1.780
_exptl_absorpt_correction_T_max 0.586
_exptl_absorpt_correction_T_min 0.498
_exptl_absorpt_correction_type 'difabs (Walker & Stuart, 1983)'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.735
_exptl_crystal_density_meas 1.732
_exptl_crystal_density_method flotation
_exptl_crystal_description block
_exptl_crystal_F_000 1712
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.30
_refine_diff_density_max 1.03
_refine_diff_density_min -0.52
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 0.825
_refine_ls_goodness_of_fit_obs 0.836
_refine_ls_hydrogen_treatment 'H atoms: see below'
_refine_ls_matrix_type full
_refine_ls_number_constraints 0
_refine_ls_number_parameters 203
_refine_ls_number_reflns 2569
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.825
_refine_ls_restrained_S_obs 0.836
_refine_ls_R_factor_all 0.0359
_refine_ls_R_factor_obs 0.0348
_refine_ls_shift/esd_max -0.001
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)]'
_refine_ls_wR_factor_all 0.0881
_refine_ls_wR_factor_obs 0.0868
_reflns_number_observed 2437
_reflns_number_total 2569
_reflns_observed_criterion >2sigma(I)
_[local]_cod_data_source_file bm1127.cif
_[local]_cod_data_source_block I
_[local]_cod_cif_authors_sg_H-M 'C 2/c'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been
'160(d)'. The value '160(d)' was changed to
'160'.
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).
'_geom_bond_publ_flag' value 'N' changed to 'n' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (20
times).
'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (33
times).
'_geom_angle_publ_flag' value 'N' changed to 'n' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (45 times).
Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana
;
_cod_database_code 2006095
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pr 0.0291(2) 0.0348(2) 0.0287(2) 0.000 -0.00330(15) 0.000
O1 0.059(2) 0.047(2) 0.057(2) -0.004(2) 0.012(2) 0.0058(15)
O2 0.098(5) 0.032(3) 0.155(6) 0.000 0.036(4) 0.000
O3 0.046(2) 0.059(2) 0.045(2) -0.0011(13) 0.000(2) -0.0003(14)
O4 0.044(2) 0.095(3) 0.045(2) 0.001(2) -0.0017(15) -0.011(2)
O5 0.066(3) 0.169(5) 0.067(3) 0.017(3) 0.025(2) -0.033(3)
O6 0.038(2) 0.046(2) 0.045(2) 0.0068(13) -0.0105(13) -0.0095(13)
O7 0.037(2) 0.037(2) 0.052(2) 0.0022(13) -0.0075(13) -0.0009(14)
O8 0.037(2) 0.103(3) 0.054(2) 0.011(2) 0.003(2) 0.000(2)
O9 0.076(3) 0.084(2) 0.041(2) 0.017(2) 0.006(2) 0.006(2)
O10 0.053(2) 0.054(2) 0.110(3) -0.014(2) -0.034(2) 0.002(2)
O11 0.124(4) 0.089(3) 0.087(3) -0.047(3) -0.050(3) 0.045(2)
O12 0.094(3) 0.092(3) 0.141(4) 0.059(3) -0.064(3) -0.065(3)
N1 0.047(4) 0.045(4) 0.072(5) 0.000 0.002(3) 0.000
N2 0.052(3) 0.076(3) 0.038(2) 0.010(2) 0.009(2) 0.005(2)
P1 0.0362(7) 0.0449(7) 0.0353(6) -0.0010(5) -0.0107(5) -0.0032(4)
P2 0.0515(8) 0.0414(7) 0.0571(7) 0.0086(5) -0.0202(6) -0.0039(5)
C1 0.033(3) 0.060(3) 0.046(3) 0.007(2) -0.015(2) -0.004(2)
C2 0.051(3) 0.073(3) 0.076(4) 0.020(3) -0.036(3) -0.006(3)
C3 0.083(5) 0.129(5) 0.054(4) 0.006(4) 0.022(3) -0.008(4)
C4 0.074(5) 0.069(4) 0.176(8) -0.023(4) 0.006(5) 0.026(5)
C5 0.127(7) 0.140(7) 0.070(4) 0.018(6) 0.015(4) 0.037(4)
C6 0.057(4) 0.096(5) 0.092(4) 0.003(3) 0.009(3) -0.038(4)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Pr 0 0.33359(3) 0.25 0.03098(14) Uani d S 0.5 Pr
O1 0.0293(2) 0.5882(3) 0.2007(2) 0.0543(8) Uani d . 1 O
O2 0 0.7941(6) 0.25 0.094(2) Uani d S 0.5 O
O3 0.1130(2) 0.3458(3) 0.1840(2) 0.0501(8) Uani d . 1 O
O4 0.0364(2) 0.2537(4) 0.1128(2) 0.0614(9) Uani d . 1 O
O5 0.1347(2) 0.2397(6) 0.0757(2) 0.1001(15) Uani d . 1 O
O6 0.08667(13) 0.4078(3) 0.3460(2) 0.0436(7) Uani d . 1 O
O7 0.06439(13) 0.1149(3) 0.2813(2) 0.0421(7) Uani d . 1 O
O8 0.2079(2) 0.2348(5) 0.2826(2) 0.0645(9) Uani d . 1 O
H8 0.1821(14) 0.284(8) 0.257(2) 0.144(8) Uiso calc R 1 H
O9 0.1231(2) 0.2960(4) 0.4760(2) 0.0671(10) Uani d . 1 O
O10 0.1956(2) 0.4631(4) 0.4090(2) 0.0734(11) Uani d . 1 O
O11 0.1018(3) -0.0175(5) 0.4052(3) 0.101(2) Uani d . 1 O
O12 0.1527(2) -0.0746(5) 0.2848(3) 0.111(2) Uani d . 1 O
N1 0 0.6598(6) 0.25 0.055(2) Uani d S 0.5 N
N2 0.0954(2) 0.2790(5) 0.1220(2) 0.0549(10) Uani d . 1 N
P1 0.14118(6) 0.34983(12) 0.39440(7) 0.0391(3) Uani d . 1 P
P2 0.11830(6) 0.05037(13) 0.32622(7) 0.0506(3) Uani d . 1 P
C1 0.1793(2) 0.1883(5) 0.3519(3) 0.0470(12) Uani d . 1 C
C2 0.2330(3) 0.1259(6) 0.4060(3) 0.068(2) Uani d . 1 C
H2A 0.2153(5) 0.096(6) 0.4542(12) 0.144(8) Uiso calc R 1 H
H2B 0.2649(13) 0.200(2) 0.416(3) 0.144(8) Uiso calc R 1 H
H2C 0.2522(17) 0.043(4) 0.3816(14) 0.144(8) Uiso calc R 1 H
C3 0.0828(3) 0.3747(8) 0.5257(3) 0.088(2) Uani d . 1 C
H3A 0.1002(14) 0.471(2) 0.535(3) 0.144(8) Uiso calc R 1 H
H3B 0.080(2) 0.323(3) 0.5742(12) 0.144(8) Uiso calc R 1 H
H3C 0.0407(7) 0.383(5) 0.5016(13) 0.144(8) Uiso calc R 1 H
C4 0.1997(3) 0.6040(7) 0.3758(5) 0.106(3) Uani d . 1 C
H4A 0.223(2) 0.5980(12) 0.3285(17) 0.144(8) Uiso calc R 1 H
H4B 0.222(2) 0.6688(16) 0.4116(13) 0.144(8) Uiso calc R 1 H
H4C 0.1573(3) 0.641(3) 0.365(3) 0.144(8) Uiso calc R 1 H
C5 0.0471(4) -0.0978(10) 0.4222(4) 0.112(3) Uani d . 1 C
H5A 0.0415(14) -0.097(5) 0.4773(5) 0.144(8) Uiso calc R 1 H
H5B 0.0519(12) -0.1975(17) 0.405(3) 0.144(8) Uiso calc R 1 H
H5C 0.0102(6) -0.054(4) 0.396(3) 0.144(8) Uiso calc R 1 H
C6 0.1453(3) -0.1070(7) 0.2034(4) 0.082(2) Uani d . 1 C
H6A 0.144(2) -0.2117(7) 0.1961(4) 0.144(8) Uiso calc R 1 H
H6B 0.1808(12) -0.067(5) 0.1766(5) 0.144(8) Uiso calc R 1 H
H6C 0.1060(11) -0.065(5) 0.1830(7) 0.144(8) Uiso calc R 1 H
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'
P P 0.1023 0.0942 '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'
Pr Pr -0.2180 2.8214 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O7 Pr O7 6_556 . 71.34(13) y
O7 Pr O6 6_556 6_556 72.34(9) n
O7 Pr O6 . 6_556 137.97(9) n
O7 Pr O6 6_556 . 137.97(9) y
O7 Pr O6 . . 72.34(9) y
O6 Pr O6 6_556 . 148.61(13) y
O7 Pr O1 6_556 6_556 132.41(10) n
O7 Pr O1 . 6_556 143.29(10) n
O6 Pr O1 6_556 6_556 78.32(10) n
O6 Pr O1 . 6_556 73.20(10) n
O7 Pr O1 6_556 . 143.29(10) y
O7 Pr O1 . . 132.41(10) y
O6 Pr O1 6_556 . 73.20(10) y
O6 Pr O1 . . 78.32(10) y
O1 Pr O1 6_556 . 49.40(15) y
O7 Pr O4 6_556 . 75.64(11) y
O7 Pr O4 . . 78.24(11) y
O6 Pr O4 6_556 . 72.87(10) y
O6 Pr O4 . . 116.42(10) y
O1 Pr O4 6_556 . 129.47(11) n
O1 Pr O4 . . 82.50(11) y
O7 Pr O4 6_556 6_556 78.24(11) n
O7 Pr O4 . 6_556 75.64(11) n
O6 Pr O4 6_556 6_556 116.42(10) n
O6 Pr O4 . 6_556 72.87(10) n
O1 Pr O4 6_556 6_556 82.50(11) n
O1 Pr O4 . 6_556 129.47(11) y
O4 Pr O4 . 6_556 147.7(2) y
O7 Pr O3 6_556 6_556 68.89(9) n
O7 Pr O3 . 6_556 115.34(10) n
O6 Pr O3 6_556 6_556 68.89(10) n
O6 Pr O3 . 6_556 109.73(10) n
O1 Pr O3 6_556 6_556 65.89(10) n
O1 Pr O3 . 6_556 109.43(10) y
O4 Pr O3 . 6_556 133.81(10) n
O4 Pr O3 6_556 6_556 48.01(10) n
O7 Pr O3 6_556 . 115.34(10) y
O7 Pr O3 . . 68.89(9) y
O6 Pr O3 6_556 . 109.73(10) y
O6 Pr O3 . . 68.89(10) y
O1 Pr O3 6_556 . 109.43(10) n
O1 Pr O3 . . 65.89(10) y
O4 Pr O3 . . 48.01(10) y
O4 Pr O3 6_556 . 133.81(10) y
O3 Pr O3 6_556 . 175.22(13) y
N1 O1 Pr . . 96.8(3) y
N2 O3 Pr . . 96.2(3) y
N2 O4 Pr . . 98.8(2) y
P1 O6 Pr . . 142.9(2) n
P2 O7 Pr . . 147.8(2) n
C3 O9 P1 . . 124.0(4) n
C4 O10 P1 . . 126.5(4) n
C5 O11 P2 . . 127.3(4) n
C6 O12 P2 . . 124.8(4) n
O2 N1 O1 . . 121.5(2) y
O2 N1 O1 . 6_556 121.5(2) n
O1 N1 O1 . 6_556 117.1(5) y
O5 N2 O4 . . 123.0(5) y
O5 N2 O3 . . 120.7(5) y
O4 N2 O3 . . 116.3(4) y
O6 P1 O10 . . 113.4(2) n
O6 P1 O9 . . 114.4(2) n
O10 P1 O9 . . 105.5(2) n
O6 P1 C1 . . 113.3(2) n
O10 P1 C1 . . 105.7(2) n
O9 P1 C1 . . 103.5(2) n
O7 P2 O12 . . 114.5(2) n
O7 P2 O11 . . 115.6(2) n
O12 P2 O11 . . 103.8(3) n
O7 P2 C1 . . 111.5(2) n
O12 P2 C1 . . 106.6(3) n
O11 P2 C1 . . 103.8(2) n
O8 C1 C2 . . 107.3(4) n
O8 C1 P2 . . 108.3(3) n
C2 C1 P2 . . 112.2(4) n
O8 C1 P1 . . 107.4(3) n
C2 C1 P1 . . 111.7(3) n
P2 C1 P1 . . 109.7(3) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pr O1 . 2.547(3) y
Pr O3 . 2.658(4) y
Pr O4 . 2.611(3) y
Pr O6 . 2.494(3) y
Pr O7 . 2.448(3) y
Pr O7 6_556 2.448(3) n
Pr O6 6_556 2.494(3) n
Pr O1 6_556 2.547(3) n
Pr O4 6_556 2.611(3) n
Pr O3 6_556 2.658(4) n
O1 N1 . 1.248(4) y
O2 N1 . 1.221(7) y
O3 N2 . 1.268(5) y
O4 N2 . 1.256(5) y
O5 N2 . 1.218(5) y
O6 P1 . 1.480(3) n
O7 P2 . 1.462(3) n
O8 C1 . 1.418(6) n
O9 C3 . 1.417(7) n
O9 P1 . 1.547(4) n
O10 C4 . 1.406(7) n
O10 P1 . 1.547(3) n
O11 C5 . 1.395(9) n
O11 P2 . 1.543(5) n
O12 C6 . 1.433(7) n
O12 P2 . 1.535(4) n
N1 O1 6_556 1.248(4) n
P1 C1 . 1.835(5) n
P2 C1 . 1.827(5) n
C1 C2 . 1.537(6) n