#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/57/1505731.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_1505731
loop_
_publ_author_name
'Lindqvist-Reis, Patric'
'Walther, Clemens'
'Klenze, Reinhardt'
'Eichhöfer, Andreas'
'Fanghänel, Thomas'
_publ_section_title
;
 Large ground-state and excited-state crystal field splitting of
 8-fold-coordinate Cm3+ in [Y(H2O)8]Cl3.15-crown-5.
;
_journal_issue                   11
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              5279
_journal_page_last               5285
_journal_paper_doi               10.1021/jp0574100
_journal_volume                  110
_journal_year                    2006
_chemical_formula_sum            'C10 H36 Cl3 O13 Y'
_chemical_formula_weight         559.65
_chemical_name_common            '[Y(H2O)8]Cl3*15-crown5'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1848(18)
_cell_length_b                   17.229(3)
_cell_length_c                   15.299(3)
_cell_measurement_temperature    200(2)
_cell_volume                     2418.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0917
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18808
_diffrn_reflns_theta_full        27.08
_diffrn_reflns_theta_max         27.08
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    2.795
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.632
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5280
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                4083
_reflns_number_total             5280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp0574100si20060123_021319.cif
_cod_data_source_block           p21n
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1505731
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Y1 Y 0.14266(3) 0.181133(18) 0.28013(2) 0.02557(12) Uani 1 1 d .
Cl1 Cl 0.64804(11) 0.16302(7) 0.33387(7) 0.0446(2) Uani 1 1 d .
Cl2 Cl 0.80624(11) 0.25296(7) 0.06225(6) 0.0437(2) Uani 1 1 d .
Cl3 Cl 0.33553(12) 0.17084(7) 0.00741(7) 0.0452(3) Uani 1 1 d .
O1 O -0.0401(3) 0.09062(18) 0.3153(2) 0.0448(7) Uani 1 1 d .
H1A H -0.143(6) 0.101(3) 0.327(4) 0.062(16) Uiso 1 1 d .
H1B H -0.042(7) 0.049(4) 0.302(4) 0.068(19) Uiso 1 1 d .
O2 O 0.3295(3) 0.1616(2) 0.3876(2) 0.0404(7) Uani 1 1 d .
H2A H 0.436(8) 0.156(4) 0.370(5) 0.08(2) Uiso 1 1 d .
H2B H 0.337(7) 0.180(3) 0.429(4) 0.055(18) Uiso 1 1 d .
O3 O 0.0643(3) 0.23038(18) 0.41467(18) 0.0381(6) Uani 1 1 d .
H3A H 0.125(6) 0.239(3) 0.458(4) 0.045(13) Uiso 1 1 d .
H3B H -0.015(5) 0.250(3) 0.428(3) 0.032(11) Uiso 1 1 d .
O4 O 0.0845(4) 0.16636(19) 0.13125(19) 0.0393(7) Uani 1 1 d .
H11A H 0.024(9) 0.187(4) 0.105(6) 0.10(3) Uiso 1 1 d .
H11B H 0.149(8) 0.167(4) 0.094(5) 0.07(2) Uiso 1 1 d .
O5 O 0.3706(3) 0.19621(18) 0.2074(2) 0.0358(6) Uani 1 1 d .
H5A H 0.451(6) 0.186(3) 0.239(4) 0.051(15) Uiso 1 1 d .
H5B H 0.379(7) 0.194(3) 0.167(4) 0.049(19) Uiso 1 1 d .
O6 O 0.2231(3) 0.05329(16) 0.2568(2) 0.0365(6) Uani 1 1 d .
H6A H 0.275(6) 0.024(4) 0.284(4) 0.060(17) Uiso 1 1 d .
H6B H 0.206(7) 0.019(4) 0.216(4) 0.070(18) Uiso 1 1 d .
O7 O -0.0887(3) 0.24570(17) 0.2563(2) 0.0353(6) Uani 1 1 d .
H7A H -0.144(8) 0.234(4) 0.284(5) 0.08(2) Uiso 1 1 d .
H7B H -0.124(6) 0.252(3) 0.209(4) 0.052(16) Uiso 1 1 d .
O8 O 0.1941(3) 0.31149(15) 0.2609(2) 0.0391(6) Uani 1 1 d D
H8A H 0.242(8) 0.334(4) 0.227(5) 0.07(2) Uiso 1 1 d .
H8B H 0.141(6) 0.348(3) 0.274(4) 0.070(19) Uiso 1 1 d D
O9 O 0.0906(3) 0.46297(19) 0.1324(2) 0.0479(7) Uani 1 1 d .
O10 O 0.3551(4) 0.3877(2) 0.1376(2) 0.0517(8) Uani 1 1 d .
O11 O 0.5550(3) 0.44816(18) 0.2685(2) 0.0486(7) Uani 1 1 d .
O12 O 0.3304(4) 0.46239(19) 0.3916(2) 0.0490(7) Uani 1 1 d .
O13 O 0.0488(3) 0.43889(16) 0.3103(2) 0.0448(7) Uani 1 1 d .
C1 C 0.1277(6) 0.4128(3) 0.0631(3) 0.0557(12) Uani 1 1 d .
H9A H 0.075(6) 0.428(3) 0.002(4) 0.066(17) Uiso 1 1 d .
H9B H 0.086(7) 0.356(4) 0.082(4) 0.077(19) Uiso 1 1 d .
C2 C 0.2894(6) 0.4116(3) 0.0559(3) 0.0598(13) Uani 1 1 d .
H10A H 0.312(4) 0.466(2) 0.037(2) 0.020(9) Uiso 1 1 d .
H10B H 0.328(7) 0.365(4) 0.004(4) 0.09(2) Uiso 1 1 d .
C3 C 0.5082(5) 0.3786(3) 0.1354(4) 0.0546(12) Uani 1 1 d .
H11B H 0.534(7) 0.328(4) 0.107(4) 0.073(19) Uiso 1 1 d .
H11A H 0.553(8) 0.415(4) 0.102(5) 0.09(2) Uiso 1 1 d .
C4 C 0.5707(5) 0.3738(3) 0.2283(4) 0.0545(12) Uani 1 1 d .
H12A H 0.479(6) 0.377(3) 0.265(3) 0.053(14) Uiso 1 1 d .
H12B H 0.695(6) 0.357(4) 0.229(4) 0.068(17) Uiso 1 1 d .
C5 C 0.5821(6) 0.4493(3) 0.3621(3) 0.0522(11) Uani 1 1 d .
H13A H 0.687(7) 0.427(4) 0.381(4) 0.08(2) Uiso 1 1 d .
H13B H 0.592(7) 0.512(4) 0.375(4) 0.08(2) Uiso 1 1 d .
C6 C 0.4566(6) 0.4172(3) 0.4121(4) 0.0548(12) Uani 1 1 d .
H14A H 0.432(7) 0.357(4) 0.386(4) 0.080(19) Uiso 1 1 d .
H14B H 0.491(7) 0.420(4) 0.478(5) 0.080(19) Uiso 1 1 d .
C7 C 0.2067(6) 0.4373(3) 0.4386(3) 0.0464(10) Uani 1 1 d .
H15A H 0.206(6) 0.379(4) 0.440(4) 0.061(16) Uiso 1 1 d .
H15B H 0.212(6) 0.455(3) 0.497(4) 0.057(15) Uiso 1 1 d .
C8 C 0.0704(6) 0.4716(3) 0.3958(3) 0.0480(10) Uani 1 1 d .
H16A H -0.027(6) 0.465(4) 0.433(4) 0.070(17) Uiso 1 1 d .
H16B H 0.077(6) 0.525(3) 0.387(3) 0.053(14) Uiso 1 1 d .
C9 C -0.0544(5) 0.4804(3) 0.2562(3) 0.0463(10) Uani 1 1 d .
H17A H -0.162(6) 0.474(3) 0.275(3) 0.051(14) Uiso 1 1 d .
H17B H -0.022(6) 0.544(3) 0.259(4) 0.060(15) Uiso 1 1 d .
C10 C -0.0506(5) 0.4495(3) 0.1644(4) 0.0508(11) Uani 1 1 d .
H18A H -0.121(6) 0.475(3) 0.118(3) 0.052(14) Uiso 1 1 d .
H18B H -0.077(6) 0.390(3) 0.161(4) 0.057(15) Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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
O8 Y1 O4 91.17(12)
O8 Y1 O2 94.67(12)
O4 Y1 O2 142.77(12)
O8 Y1 O6 145.07(11)
O4 Y1 O6 78.95(12)
O2 Y1 O6 75.36(12)
O8 Y1 O3 80.53(11)
O4 Y1 O3 145.48(11)
O2 Y1 O3 71.64(11)
O6 Y1 O3 125.22(11)
O8 Y1 O1 144.79(11)
O4 Y1 O1 91.09(13)
O2 Y1 O1 104.40(12)
O6 Y1 O1 69.52(10)
O3 Y1 O1 77.90(12)
O8 Y1 O7 73.58(11)
O4 Y1 O7 75.19(12)
O2 Y1 O7 141.52(11)
O6 Y1 O7 133.56(10)
O3 Y1 O7 70.32(11)
O1 Y1 O7 73.10(11)
O8 Y1 O5 69.70(11)
O4 Y1 O5 74.06(12)
O2 Y1 O5 73.67(12)
O6 Y1 O5 75.37(10)
O3 Y1 O5 131.57(11)
O1 Y1 O5 143.93(11)
O7 Y1 O5 130.83(11)
C1 O9 C10 114.3(4)
C3 O10 C2 113.0(4)
C4 O11 C5 115.0(4)
C6 O12 C7 112.3(4)
C9 O13 C8 113.2(3)
O9 C1 C2 109.8(4)
O10 C2 C1 108.6(4)
O10 C3 C4 108.4(4)
O11 C4 C3 108.3(4)
O11 C5 C6 113.4(4)
O12 C6 C5 108.7(4)
O12 C7 C8 108.9(4)
O13 C8 C7 108.6(4)
O13 C9 C10 108.7(4)
O9 C10 C9 109.0(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Y1 O8 2.317(3)
Y1 O4 2.328(3)
Y1 O2 2.342(3)
Y1 O6 2.356(3)
Y1 O3 2.370(3)
Y1 O1 2.372(3)
Y1 O7 2.411(3)
Y1 O5 2.433(3)
O9 C1 1.422(6)
O9 C10 1.427(6)
O10 C3 1.417(6)
O10 C2 1.423(6)
O11 C4 1.431(6)
O11 C5 1.442(6)
O12 C6 1.420(6)
O12 C7 1.440(6)
O13 C9 1.421(5)
O13 C8 1.429(6)
C1 C2 1.495(8)
C3 C4 1.509(8)
C5 C6 1.519(8)
C7 C8 1.505(7)
C9 C10 1.504(7)
