#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/78/4507851.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_4507851
loop_
_publ_author_name
'Wang, Lu-Hua'
'Shang, Ran'
'Zheng, Zhong'
'Liu, Chun-Li'
'Wang, Zhe-Ming'
_publ_section_title
;
 Two Systems of [DabcoH2]2+/[PipH2]2+--Uranyl--Oxalate Showing Reversible
 Crystal-to-Crystal Transformations Controlled by the
 Diammonium/Uranyl/Oxalate Ratios in Aqueous Solutions ([DabcoH2]2+=
 1,4-Diazabicyclo-[2.2.2]-octaneH2and [PipH2]2+= PiperazineH2)
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2597
_journal_paper_doi               10.1021/cg400364x
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C12 H22 N2 O20 U2'
_chemical_formula_weight         990.38
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 122.9686(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.9389(4)
_cell_length_b                   9.4763(2)
_cell_length_c                   14.7780(4)
_cell_measurement_reflns_used    7756
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     2460.11(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24295
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.55
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    13.242
_exptl_absorpt_correction_T_max  0.226
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995, 1997)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.00149(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2813
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0267
_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)+(0.0227P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0501
_reflns_number_gt                2032
_reflns_number_total             2813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400364x_si_001.cif
_cod_data_source_block           dabco2-290K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.3.1 from 2005-06-27.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constr.' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4507851
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_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 0.176362(10) 0.424952(19) 0.130214(15) 0.02973(9) Uani 1 1 d .
O1 O 0.15209(19) 0.2461(4) 0.1191(3) 0.0458(10) Uani 1 1 d .
O2 O 0.1989(2) 0.6033(4) 0.1369(3) 0.0495(10) Uani 1 1 d .
O3 O 0.2137(2) 0.3960(4) 0.0070(3) 0.0439(10) Uani 1 1 d D
O4 O 0.0586(2) 0.4639(4) -0.0463(3) 0.0474(10) Uani 1 1 d .
O5 O -0.06554(19) 0.5131(4) -0.1377(3) 0.0430(9) Uani 1 1 d .
O6 O 0.2119(2) 0.4291(4) 0.3110(3) 0.0458(10) Uani 1 1 d .
O7 O 0.30789(18) 0.3815(4) 0.2539(3) 0.0356(8) Uani 1 1 d .
O8 O 0.3043(2) 0.4305(5) 0.4852(3) 0.0568(12) Uani 1 1 d .
O9 O 0.4061(2) 0.3763(4) 0.4266(3) 0.0478(10) Uani 1 1 d .
C1 C -0.0018(3) 0.4918(6) -0.0523(4) 0.0351(12) Uani 1 1 d .
C2 C 0.2807(3) 0.4187(6) 0.3891(5) 0.0414(13) Uani 1 1 d .
C3 C 0.3390(3) 0.3880(6) 0.3570(4) 0.0374(13) Uani 1 1 d .
N1 N 0.4502(2) 0.3961(5) 0.6526(4) 0.0414(12) Uani 1 1 d .
H1 H 0.4136 0.3969 0.5808 0.050 Uiso 1 1 calc R
C4 C 0.5155(6) 0.3247(15) 0.6703(7) 0.195(8) Uani 1 1 d .
H41 H 0.5325 0.3678 0.6274 0.234 Uiso 1 1 calc R
H42 H 0.5031 0.2268 0.6486 0.234 Uiso 1 1 calc R
C5 C 0.4745(7) 0.5354(9) 0.6888(6) 0.157(6) Uani 1 1 d .
H51 H 0.4308 0.5958 0.6653 0.189 Uiso 1 1 calc R
H52 H 0.5024 0.5716 0.6586 0.189 Uiso 1 1 calc R
C6 C 0.4211(6) 0.3333(19) 0.7096(7) 0.239(10) Uani 1 1 d .
H61 H 0.4023 0.2394 0.6816 0.286 Uiso 1 1 calc R
H62 H 0.3791 0.3891 0.7003 0.286 Uiso 1 1 calc R
O10 O 0.1189(2) 0.2980(4) -0.1888(3) 0.0513(11) Uani 1 1 d D
H31 H 0.180(3) 0.354(6) -0.062(3) 0.077 Uiso 1 1 d D
H32 H 0.242(3) 0.462(5) -0.006(4) 0.077 Uiso 1 1 d D
H101 H 0.095(3) 0.373(4) -0.238(4) 0.077 Uiso 1 1 d D
H102 H 0.143(3) 0.241(5) -0.215(4) 0.077 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'
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
O2 U1 O1 178.19(17) . .
O2 U1 O6 90.63(16) . .
O1 U1 O6 91.11(15) . .
O2 U1 O3 87.86(17) . .
O1 U1 O3 90.92(16) . .
O6 U1 O3 147.88(13) . .
O2 U1 O7 87.66(16) . .
O1 U1 O7 93.46(14) . .
O6 U1 O7 67.05(12) . .
O3 U1 O7 80.83(13) . .
O2 U1 O4 89.93(16) . .
O1 U1 O4 88.47(15) . .
O6 U1 O4 136.02(12) . .
O3 U1 O4 76.08(13) . .
O7 U1 O4 156.86(13) . .
O2 U1 O5 89.97(16) . 5_565
O1 U1 O5 90.15(15) . 5_565
O6 U1 O5 70.57(12) . 5_565
O3 U1 O5 141.47(13) . 5_565
O7 U1 O5 137.51(12) . 5_565
O4 U1 O5 65.45(12) . 5_565
U1 O3 H31 120(3) . .
U1 O3 H32 126(4) . .
H31 O3 H32 104(3) . .
C1 O4 U1 120.0(3) . .
C1 O5 U1 120.4(3) . 5_565
C2 O6 U1 122.3(3) . .
C3 O7 U1 122.0(3) . .
O4 C1 O5 125.9(5) . .
O4 C1 C1 117.7(6) . 5_565
O5 C1 C1 116.4(6) . 5_565
O8 C2 O6 126.1(5) . .
O8 C2 C3 118.7(5) . .
O6 C2 C3 115.3(5) . .
O9 C3 O7 127.1(5) . .
O9 C3 C2 119.7(5) . .
O7 C3 C2 113.1(4) . .
C6 N1 C5 110.6(9) . .
C6 N1 C4 112.1(10) . .
C5 N1 C4 105.3(9) . .
C6 N1 H1 109.6 . .
C5 N1 H1 109.6 . .
C4 N1 H1 109.6 . .
N1 C4 C6 109.2(7) . 2_656
N1 C4 H41 109.8 . .
C6 C4 H41 109.8 2_656 .
N1 C4 H42 109.8 . .
C6 C4 H42 109.8 2_656 .
H41 C4 H42 108.3 . .
N1 C5 C5 109.0(4) . 2_656
N1 C5 H51 109.9 . .
C5 C5 H51 109.9 2_656 .
N1 C5 H52 109.9 . .
C5 C5 H52 109.9 2_656 .
H51 C5 H52 108.3 . .
N1 C6 C4 109.3(7) . 2_656
N1 C6 H61 109.8 . .
C4 C6 H61 109.8 2_656 .
N1 C6 H62 109.8 . .
C4 C6 H62 109.8 2_656 .
H61 C6 H62 108.3 . .
H101 O10 H102 107(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.743(4) .
U1 O1 1.751(4) .
U1 O6 2.352(4) .
U1 O3 2.355(4) .
U1 O7 2.370(3) .
U1 O4 2.454(4) .
U1 O5 2.454(4) 5_565
O3 H31 0.955(19) .
O3 H32 0.957(19) .
O4 C1 1.248(6) .
O5 C1 1.258(6) .
O5 U1 2.454(4) 5_565
O6 C2 1.267(6) .
O7 C3 1.293(6) .
O8 C2 1.229(7) .
O9 C3 1.212(6) .
C1 C1 1.514(10) 5_565
C2 C3 1.559(8) .
N1 C6 1.411(10) .
N1 C5 1.411(9) .
N1 C4 1.416(9) .
N1 H1 0.9100 .
C4 C6 1.535(11) 2_656
C4 H41 0.9700 .
C4 H42 0.9700 .
C5 C5 1.520(15) 2_656
C5 H51 0.9700 .
C5 H52 0.9700 .
C6 C4 1.535(11) 2_656
C6 H61 0.9700 .
C6 H62 0.9700 .
O10 H101 0.943(19) .
O10 H102 0.952(19) .
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 H1 O8 0.91 1.95 2.708(5) 139.2 .
N1 H1 O9 0.91 2.21 2.948(6) 138.1 .
O3 H31 O10 0.955(19) 1.68(2) 2.632(5) 173(5) .
O3 H32 O8 0.957(19) 1.71(2) 2.660(5) 172(6) 6_565
O10 H101 O5 0.943(19) 2.07(3) 2.976(6) 160(5) 2_554
O10 H102 O7 0.952(19) 1.84(2) 2.788(5) 174(5) 7
