#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:16:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179320 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/17/4321746.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_4321746
loop_
_publ_author_name
'P. Shiv Halasyamani'
'Robin J. Francis'
'Susan M. Walker'
'Dermot O'Hare'
_publ_contact_author_address
;
Inorganic Chemistry Laboratory
University of Oxford
South Parks Rd.
Oxford
OX1 3QR
;
_publ_contact_author_email       'dermot.ohare@chem.ox.ac.uk '
_publ_contact_author_fax         ' 01865 272 690 '
_publ_contact_author_name        'Prof. Dermot O'Hare'
_publ_contact_author_phone       ' 01865 272 658 '
_publ_section_title
;
 New Layered Uranium(VI) Molybdates: Syntheses and Structures of
 (NH₃(CH₂)₃NH₃)(H₃O)₂(UO₂)₃(MoO₄)₅,
 C(NH₂)₃(OH)(MoO₄), (C₄H₁₂N₂)(UO₂)(MoO₄)₂, and
 (C~5~H~14~N~2~)(UO~2~)(MoO~4~)~2.H~2~O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              271
_journal_page_last               279
_journal_paper_doi               10.1021/ic980836r
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'hydrothermal synthesis'
_chemical_formula_moiety         'C4 H12 U1 MO2 O10 N2'
_chemical_formula_structural     'C4 H12 U1 MO2 O10 N2'
_chemical_formula_sum            'C4 H12 Mo2 N2 O10 U'
_chemical_formula_weight         678.07
_chemical_name_systematic
;
 
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_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
_cell_angle_alpha                97.008(3)
_cell_angle_beta                 96.454(3)
_cell_angle_gamma                110.456(3)
_cell_formula_units_Z            2
_cell_length_a                   7.096(1)
_cell_length_b                   8.388(1)
_cell_length_c                   11.634(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     634.94(13)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      150.0(2)
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2439
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    14.716
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.547
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.472
_refine_diff_density_min         -2.672
_refine_diff_density_rms         0.388
_refine_ls_extinction_coef       0.029(1)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.184
_refine_ls_goodness_of_fit_obs   1.188
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2439
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_obs          0.0357
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0617P)²+0.3764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0987
_refine_ls_wR_factor_obs         0.0986
_reflns_number_observed          2413
_reflns_number_total             2439
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980836r_3.cif
_cod_data_source_block           umopiperazine
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.3764P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.3764P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        634.9(1)
_cod_database_code               4321746
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
U1 U 0.29300(3) 0.02814(3) 0.24143(2) 0.0060(2) Uani 1 d . .
Mo1 Mo 0.78681(9) 0.09174(8) 0.10407(5) 0.0062(2) Uani 1 d . .
Mo2 Mo 0.37220(9) 0.15131(8) 0.56817(5) 0.0072(2) Uani 1 d . .
O1 O 0.7972(7) -0.0038(6) -0.0381(4) 0.012(1) Uani 1 d . .
O2 O 0.2046(7) 0.0714(6) 0.4290(4) 0.0111(9) Uani 1 d . .
O3 O 0.2441(7) 0.2266(6) 0.6700(4) 0.012(1) Uani 1 d . .
O4 O 0.1567(8) -0.1981(7) 0.2291(4) 0.013(1) Uani 1 d . .
O5 O 0.9906(7) 0.0854(6) 0.2054(4) 0.014(1) Uani 1 d . .
O6 O 0.5528(7) 0.0154(6) 0.3817(4) 0.011(1) Uani 1 d . .
O7 O 0.5500(7) -0.0277(6) 0.1439(4) 0.010(1) Uani 1 d . .
O8 O 0.5853(7) 0.3265(6) 0.5592(5) 0.015(1) Uani 1 d . .
O9 O 0.4335(8) 0.2532(6) 0.2512(4) 0.012(1) Uani 1 d . .
O10 O 0.8084(8) 0.3046(7) 0.1070(5) 0.017(1) Uani 1 d . .
N1 N 0.9687(8) 0.3466(7) 0.5495(5) 0.010(1) Uani 1 d . .
H1A H 1.0189(8) 0.2666(7) 0.5823(5) 0.013 Uiso 1 calc R .
H1B H 0.8243(8) 0.3073(7) 0.5493(5) 0.013 Uiso 1 calc R .
C1 C 1.007(1) 0.3493(9) 0.4267(6) 0.013(1) Uani 1 d . .
H1C H 0.939(1) 0.2361(9) 0.3804(6) 0.017 Uiso 1 calc R .
H1D H 1.151(1) 0.3826(9) 0.4256(6) 0.017 Uiso 1 calc R .
C2 C 0.929(1) 0.4773(9) 0.3752(6) 0.015(2) Uani 1 d . .
H2A H 0.958(1) 0.4828(9) 0.2969(6) 0.019 Uiso 1 calc R .
H2B H 0.784(1) 0.4397(9) 0.3716(6) 0.019 Uiso 1 calc R .
N2 N 0.611(1) 0.5476(8) 0.1174(6) 0.015(1) Uani 1 d . .
H2C H 0.680(1) 0.6329(8) 0.1864(6) 0.02 Uiso 1 calc R .
H2D H 0.618(1) 0.4395(8) 0.1322(6) 0.02 Uiso 1 calc R .
C3 C 0.716(1) 0.598(1) 0.0165(7) 0.019(2) Uani 1 d . .
H3A H 0.854(1) 0.604(1) 0.0330(7) 0.024 Uiso 1 calc R .
H3B H 0.720(1) 0.711(1) 0.0056(7) 0.024 Uiso 1 calc R .
C4 C 0.392(1) 0.530(1) 0.0943(7) 0.019(2) Uani 1 d . .
H4A H 0.385(1) 0.640(1) 0.0861(7) 0.023 Uiso 1 calc R .
H4B H 0.327(1) 0.492(1) 0.1595(7) 0.023 Uiso 1 calc R .
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
O4 U1 O9 178.5(2) . .
O4 U1 O1 89.5(2) . 2_655
O9 U1 O1 89.7(2) . 2_655
O4 U1 O2 89.3(2) . .
O9 U1 O2 92.0(2) . .
O1 U1 O2 147.2(2) 2_655 .
O4 U1 O5 92.8(2) . 1_455
O9 U1 O5 88.2(2) . 1_455
O1 U1 O5 71.6(2) 2_655 1_455
O2 U1 O5 75.8(2) . 1_455
O4 U1 O6 90.6(2) . .
O9 U1 O6 89.2(2) . .
O1 U1 O6 140.8(2) 2_655 .
O2 U1 O6 71.9(2) . .
O5 U1 O6 147.5(2) 1_455 .
O4 U1 O7 90.3(2) . .
O9 U1 O7 88.2(2) . .
O1 U1 O7 70.5(2) 2_655 .
O2 U1 O7 142.2(2) . .
O5 U1 O7 141.9(2) 1_455 .
O6 U1 O7 70.3(2) . .
O10 Mo1 O1 110.8(2) . .
O10 Mo1 O5 109.2(2) . .
O1 Mo1 O5 109.1(2) . .
O10 Mo1 O7 109.5(2) . .
O1 Mo1 O7 108.7(2) . .
O5 Mo1 O7 109.6(2) . .
O8 Mo2 O3 106.3(2) . .
O8 Mo2 O6 110.0(2) . 2_656
O3 Mo2 O6 110.2(2) . 2_656
O8 Mo2 O2 110.9(2) . .
O3 Mo2 O2 108.4(2) . .
O6 Mo2 O2 110.9(2) 2_656 .
Mo1 O1 U1 147.1(3) . 2_655
Mo2 O2 U1 127.8(2) . .
Mo1 O5 U1 149.6(3) . 1_655
Mo2 O6 U1 136.4(2) 2_656 .
Mo1 O7 U1 138.2(2) . .
C1 N1 C2 111.6(5) . 2_766
N1 C1 C2 109.2(6) . .
N1 C2 C1 109.8(6) 2_766 .
C3 N2 C4 111.7(6) . .
N2 C3 C4 110.5(6) . 2_665
N2 C4 C3 110.0(6) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O4 1.782(5) .
U1 O9 1.782(5) .
U1 O1 2.345(5) 2_655
U1 O2 2.358(5) .
U1 O5 2.362(5) 1_455
U1 O6 2.361(4) .
U1 O7 2.401(4) .
Mo1 O10 1.733(5) .
Mo1 O1 1.768(5) .
Mo1 O5 1.780(5) .
Mo1 O7 1.776(5) .
Mo2 O8 1.725(5) .
Mo2 O3 1.758(5) .
Mo2 O6 1.797(5) 2_656
Mo2 O2 1.797(5) .
O1 U1 2.345(5) 2_655
O5 U1 2.362(5) 1_655
O6 Mo2 1.797(5) 2_656
N1 C1 1.487(9) .
N1 C2 1.505(8) 2_766
C1 C2 1.52(1) .
C2 N1 1.505(8) 2_766
N2 C3 1.48(1) .
N2 C4 1.49(1) .
C3 C4 1.51(1) 2_665
C4 C3 1.51(1) 2_665
