#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:00:38 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179648 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/01/4510125.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_4510125
loop_
_publ_author_name
'Yang, Weiting'
'Yi, Fei-Yan'
'Tian, Tao'
'Tian, Wan-Guo'
'Sun, Zhong-Ming'
_publ_section_title
;
 Structural Variation within Heterometallic Uranyl Hybrids Based on
 Flexible Alkyldiphosphonate Ligands
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1366
_journal_paper_doi               10.1021/cg401850v
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C60 H66 N8 O28 P6 U3 Zn2'
_chemical_formula_weight         2377.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.2250(10)
_cell_angle_beta                 105.5800(10)
_cell_angle_gamma                105.0420(10)
_cell_formula_units_Z            1
_cell_length_a                   12.2596(9)
_cell_length_b                   12.6030(10)
_cell_length_c                   13.0430(10)
_cell_measurement_temperature    139(2)
_cell_volume                     1816.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      139(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9384
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    7.535
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    2.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.237
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0396
_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)+(0.0327P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                4911
_reflns_number_total             6394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401850v_si_002.cif
_cod_data_source_block           pc4p-phen
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4510125
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
U1 U 0.67115(2) 0.61575(2) 0.55932(2) 0.01932(10) Uani 1 1 d .
U2 U 1.0000 1.0000 0.5000 0.01991(12) Uani 1 2 d S
Zn1 Zn 1.11418(8) 0.71502(8) 0.86902(8) 0.0256(2) Uani 1 1 d .
P1 P 0.68512(17) -0.13432(17) 0.42802(18) 0.0222(5) Uani 1 1 d .
P2 P 0.62493(18) 0.38702(17) 0.62485(18) 0.0231(5) Uani 1 1 d .
P3 P 0.99176(17) 0.75887(17) 0.63444(17) 0.0183(4) Uani 1 1 d .
O1 O 0.6769(4) -0.2306(4) 0.4829(5) 0.0283(13) Uani 1 1 d .
O2 O 0.5821(4) -0.1666(5) 0.3183(5) 0.0337(15) Uani 1 1 d .
H2C H 0.5283 -0.2248 0.3159 0.050 Uiso 1 1 calc R
O3 O 0.8006(4) -0.0924(4) 0.4035(4) 0.0275(13) Uani 1 1 d .
O4 O 0.7372(4) 0.4897(4) 0.6669(4) 0.0276(13) Uani 1 1 d .
O5 O 0.5286(4) 0.4326(4) 0.5599(4) 0.0240(13) Uani 1 1 d .
O6 O 0.5922(4) 0.3367(4) 0.7142(4) 0.0287(13) Uani 1 1 d .
O7 O 1.0917(4) 0.7780(4) 0.7412(4) 0.0264(13) Uani 1 1 d .
O8 O 0.8691(4) 0.7130(4) 0.6451(4) 0.0232(13) Uani 1 1 d .
O9 O 1.0046(4) 0.8704(4) 0.5995(4) 0.0272(13) Uani 1 1 d .
O11 O 0.6359(4) 0.6878(4) 0.6684(5) 0.0301(14) Uani 1 1 d .
O12 O 0.7053(4) 0.5422(4) 0.4518(4) 0.0283(13) Uani 1 1 d .
O13 O 1.0385(4) 0.9173(4) 0.3999(5) 0.0302(14) Uani 1 1 d .
O1W O 0.7130(6) 0.0077(6) 0.1922(6) 0.063(2) Uani 1 1 d .
O2W O 0.6832(14) 0.4428(15) 0.9269(15) 0.238(8) Uiso 1 1 d .
N1 N 1.2625(6) 0.6703(6) 0.8381(6) 0.0278(16) Uani 1 1 d .
N2 N 1.0584(6) 0.5402(6) 0.8529(5) 0.0276(16) Uani 1 1 d .
N3 N 1.2185(6) 0.8389(6) 1.0169(6) 0.0325(18) Uani 1 1 d .
N4 N 0.9805(5) 0.7570(5) 0.9288(5) 0.0240(15) Uani 1 1 d .
C1 C 0.6710(7) -0.0182(6) 0.5189(7) 0.027(2) Uani 1 1 d .
H1A H 0.5968 -0.0462 0.5368 0.032 Uiso 1 1 calc R
H1B H 0.7387 0.0048 0.5883 0.032 Uiso 1 1 calc R
C2 C 0.6678(7) 0.0870(7) 0.4755(8) 0.035(2) Uani 1 1 d .
H2A H 0.7369 0.1115 0.4495 0.043 Uiso 1 1 calc R
H2B H 0.5939 0.0684 0.4124 0.043 Uiso 1 1 calc R
C3 C 0.6719(8) 0.1836(7) 0.5652(7) 0.038(2) Uani 1 1 d .
H3A H 0.6187 0.1522 0.6058 0.045 Uiso 1 1 calc R
H3B H 0.7542 0.2157 0.6178 0.045 Uiso 1 1 calc R
C4 C 0.6354(7) 0.2771(7) 0.5235(7) 0.032(2) Uani 1 1 d .
H4A H 0.5566 0.2433 0.4652 0.039 Uiso 1 1 calc R
H4B H 0.6935 0.3129 0.4892 0.039 Uiso 1 1 calc R
C5 C 1.0057(7) 0.6576(7) 0.5276(7) 0.030(2) Uani 1 1 d .
H5A H 0.9408 0.6470 0.4587 0.036 Uiso 1 1 calc R
H5B H 1.0824 0.6908 0.5155 0.036 Uiso 1 1 calc R
C6 C 1.0013(8) 0.5426(7) 0.5486(7) 0.032(2) Uani 1 1 d .
H6A H 0.9292 0.5125 0.5690 0.038 Uiso 1 1 calc R
H6B H 1.0720 0.5513 0.6118 0.038 Uiso 1 1 calc R
C7 C 1.3585(7) 0.7351(8) 0.8228(7) 0.039(2) Uani 1 1 d .
H7A H 1.3693 0.8138 0.8305 0.047 Uiso 1 1 calc R
C8 C 1.4433(8) 0.6920(9) 0.7959(8) 0.044(3) Uani 1 1 d .
H8A H 1.5115 0.7409 0.7867 0.053 Uiso 1 1 calc R
C9 C 1.4279(8) 0.5780(9) 0.7827(8) 0.045(3) Uani 1 1 d .
H9A H 1.4867 0.5481 0.7666 0.054 Uiso 1 1 calc R
C10 C 1.3243(8) 0.5056(8) 0.7932(7) 0.034(2) Uani 1 1 d .
C11 C 1.2955(9) 0.3860(9) 0.7718(8) 0.045(3) Uani 1 1 d .
H11A H 1.3519 0.3522 0.7561 0.054 Uiso 1 1 calc R
C12 C 1.1909(9) 0.3188(8) 0.7729(7) 0.042(2) Uani 1 1 d .
H12A H 1.1726 0.2387 0.7563 0.050 Uiso 1 1 calc R
C13 C 1.1079(8) 0.3709(7) 0.7997(7) 0.029(2) Uani 1 1 d .
C14 C 0.9933(8) 0.3047(8) 0.7984(7) 0.039(2) Uani 1 1 d .
H14A H 0.9690 0.2243 0.7770 0.046 Uiso 1 1 calc R
C15 C 0.9195(8) 0.3584(8) 0.8283(8) 0.041(2) Uani 1 1 d .
H15A H 0.8445 0.3154 0.8306 0.049 Uiso 1 1 calc R
C16 C 0.9539(7) 0.4762(8) 0.8554(7) 0.036(2) Uani 1 1 d .
H16A H 0.9015 0.5123 0.8763 0.043 Uiso 1 1 calc R
C17 C 1.2444(7) 0.5572(7) 0.8201(7) 0.029(2) Uani 1 1 d .
C18 C 1.1341(7) 0.4881(7) 0.8265(6) 0.0266(19) Uani 1 1 d .
C21 C 1.3369(7) 0.8743(8) 1.0639(8) 0.044(3) Uani 1 1 d .
H21A H 1.3826 0.8360 1.0335 0.053 Uiso 1 1 calc R
C22 C 1.3962(8) 0.9658(9) 1.1560(8) 0.049(3) Uani 1 1 d .
H22A H 1.4809 0.9903 1.1858 0.059 Uiso 1 1 calc R
C23 C 1.3327(8) 1.0191(8) 1.2024(8) 0.042(2) Uani 1 1 d .
H23A H 1.3726 1.0809 1.2654 0.050 Uiso 1 1 calc R
C24 C 1.2069(8) 0.9828(7) 1.1572(7) 0.034(2) Uani 1 1 d .
C25 C 1.1330(9) 1.0315(8) 1.2027(7) 0.041(2) Uani 1 1 d .
H25A H 1.1691 1.0944 1.2651 0.049 Uiso 1 1 calc R
C26 C 1.0139(9) 0.9912(8) 1.1601(7) 0.043(2) Uani 1 1 d .
H26A H 0.9669 1.0261 1.1922 0.051 Uiso 1 1 calc R
C27 C 0.9560(8) 0.8957(7) 1.0662(7) 0.031(2) Uani 1 1 d .
C28 C 0.8322(7) 0.8453(8) 1.0208(7) 0.035(2) Uani 1 1 d .
H28A H 0.7807 0.8744 1.0516 0.042 Uiso 1 1 calc R
C29 C 0.7860(8) 0.7547(7) 0.9327(7) 0.034(2) Uani 1 1 d .
H29A H 0.7021 0.7190 0.9022 0.041 Uiso 1 1 calc R
C30 C 0.8623(7) 0.7143(7) 0.8873(7) 0.035(2) Uani 1 1 d .
H30A H 0.8282 0.6531 0.8235 0.042 Uiso 1 1 calc R
C31 C 1.1552(7) 0.8907(7) 1.0641(6) 0.0254(19) Uani 1 1 d .
C32 C 1.0265(7) 0.8462(7) 1.0168(7) 0.027(2) Uani 1 1 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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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
O12 U1 O11 179.1(3) . .
O12 U1 O8 90.1(2) . .
O11 U1 O8 90.2(2) . .
O12 U1 O1 91.9(2) . 1_565
O11 U1 O1 89.0(2) . 1_565
O8 U1 O1 82.74(18) . 1_565
O12 U1 O5 88.9(2) . 2_666
O11 U1 O5 91.1(2) . 2_666
O8 U1 O5 160.08(18) . 2_666
O1 U1 O5 77.41(17) 1_565 2_666
O12 U1 O4 87.2(2) . .
O11 U1 O4 92.0(2) . .
O8 U1 O4 77.72(18) . .
O1 U1 O4 160.43(17) 1_565 .
O5 U1 O4 122.08(17) 2_666 .
O12 U1 O5 89.4(2) . .
O11 U1 O5 89.8(2) . .
O8 U1 O5 136.03(18) . .
O1 U1 O5 141.21(17) 1_565 .
O5 U1 O5 63.8(2) 2_666 .
O4 U1 O5 58.35(16) . .
O13 U2 O13 179.999(2) 2_776 .
O13 U2 O9 90.3(2) 2_776 2_776
O13 U2 O9 89.7(2) . 2_776
O13 U2 O9 89.7(2) 2_776 .
O13 U2 O9 90.3(2) . .
O9 U2 O9 180.00(16) 2_776 .
O13 U2 O3 89.6(2) 2_776 2_766
O13 U2 O3 90.4(2) . 2_766
O9 U2 O3 91.16(19) 2_776 2_766
O9 U2 O3 88.84(19) . 2_766
O13 U2 O3 90.4(2) 2_776 1_565
O13 U2 O3 89.6(2) . 1_565
O9 U2 O3 88.84(19) 2_776 1_565
O9 U2 O3 91.16(19) . 1_565
O3 U2 O3 180.0 2_766 1_565
O7 Zn1 N2 121.4(2) . .
O7 Zn1 N3 112.8(3) . .
N2 Zn1 N3 125.3(3) . .
O7 Zn1 N4 99.5(2) . .
N2 Zn1 N4 99.1(3) . .
N3 Zn1 N4 77.9(2) . .
O7 Zn1 N1 90.1(2) . .
N2 Zn1 N1 78.6(3) . .
N3 Zn1 N1 95.2(3) . .
N4 Zn1 N1 169.8(3) . .
O1 P1 O3 114.9(3) . .
O1 P1 O2 111.3(3) . .
O3 P1 O2 107.1(3) . .
O1 P1 C1 107.2(4) . .
O3 P1 C1 108.2(3) . .
O2 P1 C1 108.0(4) . .
O6 P2 O4 113.9(3) . .
O6 P2 O5 113.3(3) . .
O4 P2 O5 103.3(3) . .
O6 P2 C4 109.1(4) . .
O4 P2 C4 111.8(4) . .
O5 P2 C4 105.0(4) . .
O8 P3 O7 112.1(3) . .
O8 P3 O9 110.2(3) . .
O7 P3 O9 109.2(3) . .
O8 P3 C5 108.2(3) . .
O7 P3 C5 109.3(4) . .
O9 P3 C5 107.7(4) . .
P1 O1 U1 175.8(4) . 1_545
P1 O3 U2 138.0(3) . 1_545
P2 O4 U1 100.4(3) . .
P2 O5 U1 145.5(3) . 2_666
P2 O5 U1 96.3(2) . .
U1 O5 U1 116.2(2) 2_666 .
P3 O7 Zn1 137.0(3) . .
P3 O8 U1 147.6(3) . .
P3 O9 U2 163.5(3) . .
C7 N1 C17 118.1(7) . .
C7 N1 Zn1 129.0(6) . .
C17 N1 Zn1 112.4(5) . .
C16 N2 C18 118.4(7) . .
C16 N2 Zn1 127.3(6) . .
C18 N2 Zn1 113.9(5) . .
C21 N3 C31 117.8(7) . .
C21 N3 Zn1 128.2(6) . .
C31 N3 Zn1 113.9(5) . .
C30 N4 C32 117.2(7) . .
C30 N4 Zn1 129.7(6) . .
C32 N4 Zn1 112.8(5) . .
C2 C1 P1 116.2(6) . .
C3 C2 C1 110.7(7) . .
C4 C3 C2 114.1(8) . .
C3 C4 P2 115.9(6) . .
C6 C5 P3 116.2(6) . .
C5 C6 C6 113.8(9) . 2_766
N1 C7 C8 122.4(9) . .
C9 C8 C7 119.5(9) . .
C8 C9 C10 119.7(9) . .
C17 C10 C9 116.3(8) . .
C17 C10 C11 119.8(8) . .
C9 C10 C11 123.8(8) . .
C12 C11 C10 122.2(8) . .
C11 C12 C13 118.4(8) . .
C18 C13 C14 116.8(8) . .
C18 C13 C12 121.7(8) . .
C14 C13 C12 121.5(8) . .
C15 C14 C13 119.2(8) . .
C14 C15 C16 120.0(9) . .
N2 C16 C15 122.2(8) . .
N1 C17 C10 123.8(8) . .
N1 C17 C18 116.7(7) . .
C10 C17 C18 119.4(8) . .
N2 C18 C13 123.3(7) . .
N2 C18 C17 118.2(7) . .
C13 C18 C17 118.4(7) . .
N3 C21 C22 122.5(9) . .
C23 C22 C21 119.7(9) . .
C22 C23 C24 119.9(8) . .
C31 C24 C23 116.4(8) . .
C31 C24 C25 120.0(8) . .
C23 C24 C25 123.6(8) . .
C26 C25 C24 121.6(8) . .
C25 C26 C27 120.8(8) . .
C28 C27 C32 116.7(7) . .
C28 C27 C26 123.9(8) . .
C32 C27 C26 119.3(8) . .
C29 C28 C27 119.6(8) . .
C28 C29 C30 119.6(8) . .
N4 C30 C29 123.2(8) . .
N3 C31 C24 123.7(8) . .
N3 C31 C32 117.1(7) . .
C24 C31 C32 119.1(7) . .
N4 C32 C27 123.5(7) . .
N4 C32 C31 117.3(7) . .
C27 C32 C31 119.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O12 1.761(5) .
U1 O11 1.777(5) .
U1 O8 2.280(5) .
U1 O1 2.310(5) 1_565
U1 O5 2.380(5) 2_666
U1 O4 2.433(6) .
U1 O5 2.510(5) .
U2 O13 1.779(5) 2_776
U2 O13 1.779(5) .
U2 O9 2.246(5) 2_776
U2 O9 2.246(5) .
U2 O3 2.306(5) 2_766
U2 O3 2.306(5) 1_565
Zn1 O7 1.943(6) .
Zn1 N2 2.087(7) .
Zn1 N3 2.114(7) .
Zn1 N4 2.140(6) .
Zn1 N1 2.154(6) .
P1 O1 1.499(6) .
P1 O3 1.515(5) .
P1 O2 1.544(6) .
P1 C1 1.807(8) .
P2 O6 1.510(6) .
P2 O4 1.521(5) .
P2 O5 1.554(5) .
P2 C4 1.811(8) .
P3 O8 1.517(5) .
P3 O7 1.524(5) .
P3 O9 1.529(6) .
P3 C5 1.808(8) .
O1 U1 2.310(5) 1_545
O3 U2 2.306(5) 1_545
O5 U1 2.380(5) 2_666
N1 C7 1.332(10) .
N1 C17 1.355(10) .
N2 C16 1.337(10) .
N2 C18 1.351(10) .
N3 C21 1.334(10) .
N3 C31 1.341(10) .
N4 C30 1.328(10) .
N4 C32 1.345(9) .
C1 C2 1.528(11) .
C2 C3 1.527(11) .
C3 C4 1.494(12) .
C5 C6 1.508(11) .
C6 C6 1.511(15) 2_766
C7 C8 1.388(12) .
C8 C9 1.375(14) .
C9 C10 1.413(12) .
C10 C17 1.396(11) .
C10 C11 1.418(13) .
C11 C12 1.346(12) .
C12 C13 1.434(11) .
C13 C18 1.392(11) .
C13 C14 1.430(11) .
C14 C15 1.360(12) .
C15 C16 1.390(12) .
C17 C18 1.437(11) .
C21 C22 1.397(12) .
C22 C23 1.348(12) .
C23 C24 1.413(12) .
C24 C31 1.406(11) .
C24 C25 1.418(12) .
C25 C26 1.337(12) .
C26 C27 1.439(11) .
C27 C28 1.398(11) .
C27 C32 1.414(11) .
C28 C29 1.357(11) .
C29 C30 1.390(11) .
C31 C32 1.446(11) .
