#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:21:30 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179574 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/39/4503970.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_4503970
loop_
_publ_author_name
'Tang, Si-Fu'
'Song, Jun-Ling'
'Li, Xiu-Ling'
'Mao, Jiang-Gao'
_publ_section_title
;
 Novel Luminescent Lanthanide(III) Diphosphonates with Rarely Observed
 Topology
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              360
_journal_paper_doi               10.1021/cg060590y
_journal_volume                  7
_journal_year                    2007
_chemical_formula_sum            'C12 H25 Eu N4 O16 P4'
_chemical_formula_weight         757.20
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 92.294(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6305(5)
_cell_length_b                   17.0798(8)
_cell_length_c                   16.7882(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3045.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury CCD''
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23192
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    2.337
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8844
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1500
_refine_diff_density_max         1.764
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.154
_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     342
_refine_ls_number_reflns         6937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0641P)²+12.4837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                5997
_reflns_number_total             6937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg060590ysi20061101_042306.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4503970
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
Eu1 Eu 0.71526(2) 0.002683(13) 0.485873(13) 0.01749(10) Uani 1 1 d .
P1 P 0.45356(12) -0.01422(8) 0.33685(8) 0.0236(3) Uani 1 1 d .
P2 P 0.47654(12) 0.14016(8) 0.42188(8) 0.0243(3) Uani 1 1 d .
P3 P 1.00190(11) -0.10979(7) 0.43321(8) 0.0213(3) Uani 1 1 d .
P4 P 0.93565(13) 0.03161(9) 0.32328(8) 0.0271(3) Uani 1 1 d .
N1 N 0.5923(4) 0.1052(3) 0.2854(3) 0.0278(9) Uani 1 1 d .
H1B H 0.6494 0.1157 0.3250 0.033 Uiso 1 1 calc R
H1C H 0.6138 0.0584 0.2654 0.033 Uiso 1 1 calc R
N2 N 0.7321(4) 0.1576(3) 0.1995(3) 0.0286(9) Uani 1 1 d .
N3 N 1.1073(4) -0.0820(3) 0.2936(3) 0.0284(10) Uani 1 1 d .
H3B H 1.1305 -0.0346 0.2760 0.034 Uiso 1 1 calc R
H3C H 1.1637 -0.0953 0.3328 0.034 Uiso 1 1 calc R
N4 N 1.2442(4) -0.1379(3) 0.2086(3) 0.0331(10) Uani 1 1 d .
C1 C 0.4733(5) 0.0922(3) 0.3245(3) 0.0272(11) Uani 1 1 d .
H1A H 0.4035 0.1130 0.2910 0.033 Uiso 1 1 calc R
C2 C 0.6133(5) 0.1572(3) 0.2284(3) 0.0258(10) Uani 1 1 d .
C3 C 0.5262(5) 0.2111(3) 0.1951(3) 0.0339(12) Uani 1 1 d .
H3A H 0.4439 0.2116 0.2118 0.041 Uiso 1 1 calc R
C4 C 0.5625(6) 0.2627(4) 0.1383(4) 0.0400(14) Uani 1 1 d .
H4A H 0.5046 0.2987 0.1173 0.048 Uiso 1 1 calc R
C5 C 0.6850(6) 0.2622(4) 0.1111(4) 0.0408(14) Uani 1 1 d .
H5A H 0.7093 0.2973 0.0722 0.049 Uiso 1 1 calc R
C6 C 0.7677(6) 0.2091(4) 0.1431(4) 0.0377(13) Uani 1 1 d .
H6A H 0.8498 0.2080 0.1260 0.045 Uiso 1 1 calc R
C11 C 0.9865(5) -0.0708(3) 0.3319(3) 0.0268(11) Uani 1 1 d .
H11A H 0.9236 -0.1027 0.3026 0.032 Uiso 1 1 calc R
C12 C 1.1242(5) -0.1316(3) 0.2343(3) 0.0264(10) Uani 1 1 d .
C13 C 1.2732(7) -0.1890(4) 0.1499(4) 0.0463(16) Uani 1 1 d .
H13A H 1.3561 -0.1919 0.1343 0.056 Uiso 1 1 calc R
C14 C 1.1878(8) -0.2350(5) 0.1141(5) 0.062(2) Uani 1 1 d .
H14A H 1.2098 -0.2698 0.0744 0.074 Uiso 1 1 calc R
C15 C 1.0651(8) -0.2296(5) 0.1377(5) 0.065(2) Uani 1 1 d .
H15A H 1.0035 -0.2608 0.1128 0.077 Uiso 1 1 calc R
C16 C 1.0317(6) -0.1792(4) 0.1971(4) 0.0495(18) Uani 1 1 d .
H16A H 0.9487 -0.1766 0.2124 0.059 Uiso 1 1 calc R
O11 O 0.5709(4) -0.0390(2) 0.3848(2) 0.0328(8) Uani 1 1 d .
O12 O 0.4456(4) -0.0514(3) 0.2552(2) 0.0367(9) Uani 1 1 d .
O13 O 0.3331(4) -0.0260(2) 0.3811(2) 0.0297(8) Uani 1 1 d .
O21 O 0.4824(4) 0.2300(2) 0.4069(3) 0.0391(10) Uani 1 1 d .
H21A H 0.4131 0.2456 0.3905 0.059 Uiso 1 1 calc R
O22 O 0.5976(3) 0.1157(2) 0.4634(2) 0.0282(8) Uani 1 1 d .
O23 O 0.3579(3) 0.1196(2) 0.4639(2) 0.0290(8) Uani 1 1 d .
O31 O 0.9932(4) -0.2006(2) 0.4238(3) 0.0378(10) Uani 1 1 d .
H31A H 0.9208 -0.2149 0.4308 0.057 Uiso 1 1 calc R
O32 O 1.1300(3) -0.0892(2) 0.4658(2) 0.0275(8) Uani 1 1 d .
O33 O 0.8937(3) -0.0803(2) 0.4812(2) 0.0241(7) Uani 1 1 d .
O41 O 0.9246(4) 0.0539(3) 0.2372(2) 0.0431(11) Uani 1 1 d .
O42 O 1.0478(4) 0.0813(2) 0.3614(2) 0.0333(9) Uani 1 1 d .
H42A H 1.0522 0.0741 0.4097 0.050 Uiso 1 1 calc R
O43 O 0.8167(3) 0.0400(2) 0.3672(2) 0.0292(8) Uani 1 1 d .
O1W O 0.7154(7) -0.1508(5) 0.2977(6) 0.126(4) Uani 1 1 d .
O2W O 0.7579(6) -0.2401(4) 0.4455(5) 0.101(3) Uani 1 1 d .
O3W O 1.1950(12) 0.1726(9) 0.2454(11) 0.112(6) Uani 0.50 1 d P
O4W O 0.2807(10) 0.2972(9) 0.3564(10) 0.107(6) Uani 0.50 1 d P
O5W O 0.487(2) 0.0047(11) 0.1149(14) 0.137(8) Uiso 0.50 1 d P
O6W O 0.573(4) 0.096(2) 0.013(2) 0.247(14) Uiso 0.50 1 d P
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'
Eu Eu -0.1578 3.6682 '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
O22 Eu1 O32 84.16(13) . 3_756
O22 Eu1 O13 82.91(14) . 3_656
O32 Eu1 O13 74.90(13) 3_756 3_656
O22 Eu1 O11 78.61(13) . .
O32 Eu1 O11 150.87(13) 3_756 .
O13 Eu1 O11 125.21(14) 3_656 .
O22 Eu1 O33 156.58(13) . .
O32 Eu1 O33 80.57(12) 3_756 .
O13 Eu1 O33 109.80(13) 3_656 .
O11 Eu1 O33 107.16(13) . .
O22 Eu1 O43 84.33(13) . .
O32 Eu1 O43 77.64(13) 3_756 .
O13 Eu1 O43 150.69(14) 3_656 .
O11 Eu1 O43 77.44(13) . .
O33 Eu1 O43 75.15(12) . .
O22 Eu1 O23 126.98(13) . 3_656
O32 Eu1 O23 131.65(13) 3_756 3_656
O13 Eu1 O23 74.10(13) 3_656 3_656
O11 Eu1 O23 77.17(13) . 3_656
O33 Eu1 O23 76.22(12) . 3_656
O43 Eu1 O23 133.64(13) . 3_656
O22 Eu1 P1 78.61(10) . 3_656
O32 Eu1 P1 92.65(9) 3_756 3_656
O13 Eu1 P1 18.70(9) 3_656 3_656
O11 Eu1 P1 106.55(10) . 3_656
O33 Eu1 P1 119.59(9) . 3_656
O43 Eu1 P1 161.17(10) . 3_656
O23 Eu1 P1 64.52(9) 3_656 3_656
O22 Eu1 P2 108.95(10) . 3_656
O32 Eu1 P2 133.50(9) 3_756 3_656
O13 Eu1 P2 63.41(10) 3_656 3_656
O11 Eu1 P2 74.85(10) . 3_656
O33 Eu1 P2 94.43(9) . 3_656
O43 Eu1 P2 145.90(10) . 3_656
O23 Eu1 P2 18.60(9) 3_656 3_656
P1 Eu1 P2 49.95(3) 3_656 3_656
O22 Eu1 P2 15.89(9) . .
O32 Eu1 P2 99.80(9) 3_756 .
O13 Eu1 P2 89.70(10) 3_656 .
O11 Eu1 P2 63.19(10) . .
O33 Eu1 P2 159.66(9) . .
O43 Eu1 P2 85.03(9) . .
O23 Eu1 P2 116.11(9) 3_656 .
P1 Eu1 P2 80.75(3) 3_656 .
P2 Eu1 P2 99.64(3) 3_656 .
O12 P1 O11 112.3(2) . .
O12 P1 O13 111.8(2) . .
O11 P1 O13 113.2(2) . .
O12 P1 C1 108.4(2) . .
O11 P1 C1 103.9(2) . .
O13 P1 C1 106.7(2) . .
O12 P1 Eu1 140.75(16) . 3_656
O11 P1 Eu1 90.15(16) . 3_656
O13 P1 Eu1 29.68(15) . 3_656
C1 P1 Eu1 95.96(17) . 3_656
O22 P2 O23 115.8(2) . .
O22 P2 O21 108.1(2) . .
O23 P2 O21 110.1(2) . .
O22 P2 C1 106.0(2) . .
O23 P2 C1 109.1(2) . .
O21 P2 C1 107.3(2) . .
O22 P2 Eu1 95.85(16) . 3_656
O23 P2 Eu1 30.36(14) . 3_656
O21 P2 Eu1 140.40(16) . 3_656
C1 P2 Eu1 95.21(16) . 3_656
O22 P2 Eu1 25.12(14) . .
O23 P2 Eu1 107.52(15) . .
O21 P2 Eu1 131.36(16) . .
C1 P2 Eu1 87.83(17) . .
Eu1 P2 Eu1 80.36(3) 3_656 .
O32 P3 O33 115.4(2) . .
O32 P3 O31 108.8(2) . .
O33 P3 O31 109.9(2) . .
O32 P3 C11 107.6(2) . .
O33 P3 C11 109.4(2) . .
O31 P3 C11 105.4(2) . .
O41 P4 O43 114.7(2) . .
O41 P4 O42 106.5(2) . .
O43 P4 O42 112.9(2) . .
O41 P4 C11 109.3(3) . .
O43 P4 C11 107.7(2) . .
O42 P4 C11 105.3(2) . .
C2 N1 C1 126.6(4) . .
C6 N2 C2 122.5(5) . .
C12 N3 C11 124.0(4) . .
C13 N4 C12 121.3(5) . .
N1 C1 P2 110.3(4) . .
N1 C1 P1 107.7(4) . .
P2 C1 P1 109.9(3) . .
N1 C2 N2 116.2(5) . .
N1 C2 C3 126.6(5) . .
N2 C2 C3 117.2(5) . .
C4 C3 C2 120.1(5) . .
C3 C4 C5 121.1(6) . .
C6 C5 C4 118.1(5) . .
N2 C6 C5 121.0(6) . .
N3 C11 P3 108.2(4) . .
N3 C11 P4 110.4(4) . .
P3 C11 P4 115.9(3) . .
N3 C12 N4 116.3(5) . .
N3 C12 C16 126.2(5) . .
N4 C12 C16 117.4(5) . .
C14 C13 N4 122.5(6) . .
C13 C14 C15 117.9(6) . .
C16 C15 C14 121.6(7) . .
C15 C16 C12 119.3(6) . .
P1 O11 Eu1 142.9(2) . .
P1 O12 O5W 131.5(5) . .
P1 O13 Eu1 131.6(2) . 3_656
P2 O21 O4W 117.3(4) . .
P2 O22 Eu1 139.0(2) . .
P2 O23 Eu1 131.0(2) . 3_656
P3 O31 O2W 107.1(2) . .
P3 O32 Eu1 154.1(2) . 3_756
P3 O33 Eu1 147.2(2) . .
P4 O43 Eu1 143.5(2) . .
O6W O5W O12 157.6(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Eu1 O22 2.322(3) .
Eu1 O32 2.333(4) 3_756
Eu1 O13 2.346(4) 3_656
Eu1 O11 2.352(4) .
Eu1 O33 2.372(3) .
Eu1 O43 2.389(3) .
Eu1 O23 2.394(4) 3_656
Eu1 P1 3.5419(13) 3_656
Eu1 P2 3.5722(13) 3_656
Eu1 P2 3.5902(13) .
P1 O12 1.511(4) .
P1 O11 1.518(4) .
P1 O13 1.519(4) .
P1 C1 1.842(6) .
P1 Eu1 3.5419(13) 3_656
P2 O22 1.498(4) .
P2 O23 1.511(4) .
P2 O21 1.557(4) .
P2 C1 1.828(6) .
P2 Eu1 3.5722(13) 3_656
P3 O32 1.489(4) .
P3 O33 1.516(3) .
P3 O31 1.562(4) .
P3 C11 1.827(6) .
P4 O41 1.495(4) .
P4 O43 1.497(4) .
P4 O42 1.578(4) .
P4 C11 1.835(6) .
N1 C2 1.331(6) .
N1 C1 1.464(6) .
N2 C6 1.357(7) .
N2 C2 1.371(6) .
N3 C12 1.325(6) .
N3 C11 1.471(6) .
N4 C13 1.362(7) .
N4 C12 1.367(7) .
C2 C3 1.405(7) .
C3 C4 1.365(8) .
C4 C5 1.397(9) .
C5 C6 1.358(9) .
C12 C16 1.403(8) .
C13 C14 1.326(11) .
C14 C15 1.382(11) .
C15 C16 1.374(9) .
O12 O5W 2.60(2) .
O13 Eu1 2.346(4) 3_656
O21 O4W 2.547(10) .
O23 Eu1 2.394(4) 3_656
O31 O2W 2.630(7) .
O32 Eu1 2.333(4) 3_756
O1W O4W 2.738(17) 2_645
O5W O6W 2.52(4) .
