#------------------------------------------------------------------------------
#$Date: 2019-11-25 02:08:40 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239937 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/05/4350547.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_4350547
loop_
_publ_author_name
'Luo, Junjian'
'Xu, Li'
_publ_section_title
;
 Layered lanthanide molybdate pillared by chiral [lambda-Mo2O4EDTA]2-.
;
_journal_issue                   26
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11030
_journal_page_last               11034
_journal_paper_doi               10.1021/ic0611793
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C10 H16 Eu2 Mo4 N2 O22'
_chemical_formula_weight         1203.93
_chemical_name_common            '[(H2O)EuMoO4][Mo2O4EDTA]'
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2 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                 109.823(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3383(18)
_cell_length_b                   10.5558(12)
_cell_length_c                   12.0715(18)
_cell_measurement_reflns_used    1908
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.8487
_cell_volume                     1239.3(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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4628
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    7.049
_exptl_absorpt_correction_T_max  0.3635
_exptl_absorpt_correction_T_min  0.2615
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange-redish
_exptl_crystal_density_diffrn    3.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.429
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2487
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0208
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0396
_reflns_number_gt                2422
_reflns_number_total             2487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0611793si20060628_111735.cif
_cod_data_source_block           '[(H2O)EuMoO4][Mo2O4EDTA]_(2)'
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4350547
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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
Eu Eu 0.28637(2) 1.04077(3) 0.62674(2) 0.00834(6) Uani 1 1 d .
Mo1 Mo 0.0000 0.78406(7) 0.5000 0.01000(17) Uani 1 2 d S
Mo2 Mo 0.0000 1.29034(6) 0.5000 0.01050(18) Uani 1 2 d S
Mo3 Mo 0.11032(5) 0.89925(6) 0.08997(5) 0.01387(11) Uani 1 1 d .
O1 O 0.1283(6) 0.8788(5) 0.5983(5) 0.0252(12) Uani 1 1 d .
O2 O 0.0727(5) 0.6858(5) 0.4185(5) 0.0280(12) Uani 1 1 d .
O3 O 0.1197(5) 1.1948(5) 0.6064(4) 0.0196(11) Uani 1 1 d .
O4 O 0.0875(5) 1.3841(5) 0.4289(4) 0.0240(12) Uani 1 1 d .
O5 O 0.1602(5) 0.9341(4) 0.2701(4) 0.0258(12) Uani 1 1 d .
O6 O 0.1753(4) 1.0612(6) 0.4198(3) 0.0311(13) Uani 1 1 d .
O7 O 0.3177(5) 0.9264(5) 0.1167(4) 0.0289(13) Uani 1 1 d .
O8 O 0.4913(3) 1.0333(8) 0.7924(3) 0.0351(12) Uani 1 1 d .
O9 O 0.1338(5) 0.7404(5) 0.1056(4) 0.0338(12) Uani 1 1 d .
O10 O -0.0782(4) 0.9365(4) 0.0756(3) 0.0162(9) Uani 1 1 d .
O11 O 0.2476(6) 1.0072(5) 0.8119(4) 0.0328(15) Uani 1 1 d .
N1 N 0.1475(5) 1.1248(5) 0.1246(4) 0.0128(11) Uani 1 1 d .
C1 C 0.1510(5) 1.0409(10) 0.3135(4) 0.0165(10) Uani 1 1 d .
C2 C 0.1051(7) 1.1501(6) 0.2279(5) 0.0189(14) Uani 1 1 d .
H2A H 0.0059 1.1591 0.2029 0.023 Uiso 1 1 calc R
H2B H 0.1465 1.2283 0.2657 0.023 Uiso 1 1 calc R
C3 C 0.3808(5) 1.0298(10) 0.1640(4) 0.0261(16) Uani 1 1 d .
C4 C 0.2996(6) 1.1452(7) 0.1596(6) 0.0234(16) Uani 1 1 d .
H4A H 0.3168 1.2038 0.1043 0.028 Uiso 1 1 calc R
H4B H 0.3317 1.1849 0.2367 0.028 Uiso 1 1 calc R
C5 C 0.0774(6) 1.2159(6) 0.0260(5) 0.0174(13) Uani 1 1 d .
H5B H 0.1062 1.3009 0.0544 0.026 Uiso 1 1 calc R
H5C H 0.1127 1.1996 -0.0376 0.026 Uiso 1 1 calc R
H6B H 0.295(7) 1.051(9) 0.851(5) 0.02(2) Uiso 1 1 d .
H6A H 0.180(10) 1.005(13) 0.835(9) 0.12(5) 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'
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'
Mo Mo -1.6832 0.6857 '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
O2 Eu O1 158.38(19) 4_556 .
O2 Eu O3 90.9(2) 4_556 .
O1 Eu O3 92.32(14) . .
O2 Eu O4 86.74(14) 4_556 4_546
O1 Eu O4 82.5(2) . 4_546
O3 Eu O4 158.50(16) . 4_546
O2 Eu O8 76.5(2) 4_556 .
O1 Eu O8 119.1(2) . .
O3 Eu O8 122.1(2) . .
O4 Eu O8 78.1(2) 4_546 .
O2 Eu O6 79.03(19) 4_556 .
O1 Eu O6 81.12(19) . .
O3 Eu O6 75.45(17) . .
O4 Eu O6 83.13(18) 4_546 .
O8 Eu O6 149.75(15) . .
O2 Eu O11 129.12(19) 4_556 .
O1 Eu O11 72.49(18) . .
O3 Eu O11 81.44(18) . .
O4 Eu O11 116.29(19) 4_546 .
O8 Eu O11 66.28(16) . .
O6 Eu O11 143.96(17) . .
O1 Mo1 O1 110.8(4) . 2_556
O1 Mo1 O2 110.1(3) . .
O1 Mo1 O2 108.9(2) 2_556 .
O1 Mo1 O2 108.9(2) . 2_556
O1 Mo1 O2 110.1(3) 2_556 2_556
O2 Mo1 O2 107.9(4) . 2_556
O4 Mo2 O4 111.1(4) . 2_556
O4 Mo2 O3 108.5(2) . 2_556
O4 Mo2 O3 109.2(2) 2_556 2_556
O4 Mo2 O3 109.2(2) . .
O4 Mo2 O3 108.5(2) 2_556 .
O3 Mo2 O3 110.4(3) 2_556 .
O9 Mo3 O10 108.2(2) . .
O9 Mo3 O10 106.3(2) . 2
O10 Mo3 O10 92.92(17) . 2
O9 Mo3 O7 91.0(2) . .
O10 Mo3 O7 160.05(18) . .
O10 Mo3 O7 86.53(18) 2 .
O9 Mo3 O5 94.7(2) . .
O10 Mo3 O5 86.73(18) . .
O10 Mo3 O5 157.85(17) 2 .
O7 Mo3 O5 86.4(2) . .
O9 Mo3 N1 160.6(2) . .
O10 Mo3 N1 84.95(17) . .
O10 Mo3 N1 86.60(16) 2 .
O7 Mo3 N1 75.10(18) . .
O5 Mo3 N1 71.29(17) . .
O9 Mo3 Mo3 98.45(17) . 2
O10 Mo3 Mo3 49.05(11) . 2
O10 Mo3 Mo3 48.58(12) 2 2
O7 Mo3 Mo3 135.02(15) . 2
O5 Mo3 Mo3 135.78(14) . 2
N1 Mo3 Mo3 100.93(11) . 2
Mo1 O1 Eu 148.7(3) . .
Mo1 O2 Eu 161.2(3) . 4_546
Mo2 O3 Eu 142.1(3) . .
Mo2 O4 Eu 166.2(3) . 4_556
C1 O5 Mo3 124.3(4) . .
C1 O6 Eu 158.0(5) . .
C3 O7 Mo3 121.4(4) . .
C3 O8 Eu 150.8(4) 2_656 .
Mo3 O10 Mo3 82.37(15) . 2
C2 N1 C4 108.6(5) . .
C2 N1 C5 110.4(5) . .
C4 N1 C5 107.9(4) . .
C2 N1 Mo3 104.3(4) . .
C4 N1 Mo3 106.2(4) . .
C5 N1 Mo3 118.9(3) . .
O6 C1 O5 124.6(8) . .
O6 C1 C2 118.8(8) . .
O5 C1 C2 116.6(4) . .
N1 C2 C1 108.9(5) . .
O8 C3 O7 120.8(9) 2_656 .
O8 C3 C4 120.1(9) 2_656 .
O7 C3 C4 119.0(5) . .
C3 C4 N1 115.0(6) . .
C5 C5 N1 119.0(5) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Eu O2 2.303(5) 4_556
Eu O1 2.309(5) .
Eu O3 2.320(5) .
Eu O4 2.341(5) 4_546
Eu O8 2.371(4) .
Eu O6 2.379(4) .
Eu O11 2.427(5) .
Mo1 O1 1.761(5) .
Mo1 O1 1.761(5) 2_556
Mo1 O2 1.763(5) .
Mo1 O2 1.763(5) 2_556
Mo2 O4 1.750(5) .
Mo2 O4 1.750(5) 2_556
Mo2 O3 1.767(5) 2_556
Mo2 O3 1.767(5) .
Mo3 O9 1.695(5) .
Mo3 O10 1.938(4) .
Mo3 O10 1.952(4) 2
Mo3 O7 2.077(5) .
Mo3 O5 2.091(5) .
Mo3 N1 2.425(5) .
Mo3 Mo3 2.5614(11) 2
O2 Eu 2.303(5) 4_546
O4 Eu 2.341(5) 4_556
O5 C1 1.260(10) .
O6 C1 1.240(6) .
O7 C3 1.300(11) .
O8 C3 1.247(6) 2_656
O10 Mo3 1.952(4) 2
N1 C2 1.479(8) .
N1 C4 1.499(7) .
N1 C5 1.511(7) .
C1 C2 1.513(10) .
C3 O8 1.247(6) 2_656
C3 C4 1.470(12) .
C5 C5 1.508(11) 2
