#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:59:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179224 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/46/4314633.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_4314633
loop_
_publ_author_name
'Tian-Hua Zhou'
'Fei-Yan Yi'
'Pei-Xin Li'
'Jiang-Gao Mao'
_publ_section_title
;
 Synthesis, Crystal Structures, and Luminescent Properties of Two Series'
 of New Lanthanide (III) Amino-Carboxylate-Phosphonates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              905
_journal_page_last               915
_journal_paper_doi               10.1021/ic901621x
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C9 H14 Cl Eu N O7 P'
_chemical_formula_sum            'C9 H14 Cl Eu N O7 P'
_chemical_formula_weight         466.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.496(2)
_cell_length_b                   6.8277(6)
_cell_length_c                   8.7335(8)
_cell_measurement_reflns_used    3514
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4642
_cell_measurement_theta_min      2.5116
_cell_volume                     1401.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10508
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    4.810
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6023
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.866
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00036(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0283P)²+1.0234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0604
_reflns_number_gt                1543
_reflns_number_total             1740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901621x_si_001_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314633
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.291287(10) 0.2500 0.65832(3) 0.01517(10) Uani 1 2 d S . .
Cl1 Cl 0.40791(7) 0.2500 0.5667(2) 0.0608(6) Uani 1 2 d S . .
P1 P 0.20951(5) 0.2500 1.02052(15) 0.0153(3) Uani 1 2 d S . .
N1 N 0.09924(18) 0.2500 1.1366(5) 0.0226(10) Uani 1 2 d S . .
H1B H 0.1077 0.3570 1.1923 0.027 Uiso 1 1 d R . .
C1 C 0.1332(2) 0.2500 0.9922(6) 0.0315(14) Uani 1 2 d S . .
H1A H 0.1229 0.1364 0.9336 0.038 Uiso 1 1 d R . .
C2 C 0.0375(2) 0.2500 1.0978(7) 0.056(2) Uani 1 2 d S . .
H2A H 0.0295 0.1364 1.0368 0.067 Uiso 1 1 d R . .
C3 C -0.0020(2) 0.2500 1.2363(7) 0.0420(19) Uani 1 2 d S . .
C4 C -0.0224(2) 0.4236(9) 1.2938(5) 0.0493(14) Uani 1 1 d . . .
H4A H -0.0075 0.5450 1.2557 0.059 Uiso 1 1 d R . .
C5 C -0.0646(2) 0.4252(8) 1.4062(5) 0.0435(12) Uani 1 1 d . . .
H5A H -0.0791 0.5464 1.4457 0.052 Uiso 1 1 d R . .
C6 C -0.0859(2) 0.2500 1.4616(6) 0.0332(15) Uani 1 2 d S . .
C7 C -0.1306(2) 0.2500 1.5841(6) 0.0268(13) Uani 1 2 d S . .
O1 O 0.23208(18) 0.2500 0.8603(4) 0.0353(11) Uani 1 2 d S . .
O2 O 0.22379(13) 0.0704(4) 1.1124(4) 0.0322(7) Uani 1 1 d . . .
O3 O -0.14878(12) 0.4122(4) 1.6356(3) 0.0337(7) Uani 1 1 d . . .
O1W O 0.19389(19) 0.2500 0.5355(6) 0.0412(11) Uani 1 2 d S . .
H1WA H 0.1903 0.3516 0.4801 0.062 Uiso 1 1 d R . .
O2W O 0.2993(2) 0.2500 0.3684(5) 0.0481(13) Uani 1 2 d S . .
H2WA H 0.3173 0.3516 0.3399 0.072 Uiso 1 1 d 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 0.0000 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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 Eu1 O2 92.44(8) . 2_554 ?
O1 Eu1 O2 92.44(8) . 8_665 ?
O2 Eu1 O2 152.50(16) 2_554 8_665 ?
O1 Eu1 O1W 76.86(15) . . ?
O2 Eu1 O1W 77.41(8) 2_554 . ?
O2 Eu1 O1W 77.41(8) 8_665 . ?
O1 Eu1 O2W 146.01(15) . . ?
O2 Eu1 O2W 80.44(8) 2_554 . ?
O2 Eu1 O2W 80.44(8) 8_665 . ?
O1W Eu1 O2W 69.14(16) . . ?
O1 Eu1 O3 77.69(12) . 6_658 ?
O2 Eu1 O3 129.58(10) 2_554 6_658 ?
O2 Eu1 O3 77.87(11) 8_665 6_658 ?
O1W Eu1 O3 143.41(10) . 6_658 ?
O2W Eu1 O3 131.73(12) . 6_658 ?
O1 Eu1 O3 77.69(12) . 4_557 ?
O2 Eu1 O3 77.87(11) 2_554 4_557 ?
O2 Eu1 O3 129.58(11) 8_665 4_557 ?
O1W Eu1 O3 143.41(10) . 4_557 ?
O2W Eu1 O3 131.73(12) . 4_557 ?
O3 Eu1 O3 51.71(13) 6_658 4_557 ?
O1 Eu1 Cl1 144.53(12) . . ?
O2 Eu1 Cl1 95.80(8) 2_554 . ?
O2 Eu1 Cl1 95.80(8) 8_665 . ?
O1W Eu1 Cl1 138.60(12) . . ?
O2W Eu1 Cl1 69.46(12) . . ?
O3 Eu1 Cl1 70.51(7) 6_658 . ?
O3 Eu1 Cl1 70.51(7) 4_557 . ?
O1 Eu1 C7 77.47(15) . 6_658 ?
O2 Eu1 C7 103.74(8) 2_554 6_658 ?
O2 Eu1 C7 103.74(8) 8_665 6_658 ?
O1W Eu1 C7 154.33(16) . 6_658 ?
O2W Eu1 C7 136.52(16) . 6_658 ?
O3 Eu1 C7 25.88(7) 6_658 6_658 ?
O3 Eu1 C7 25.88(7) 4_557 6_658 ?
Cl1 Eu1 C7 67.06(11) . 6_658 ?
O1 P1 O2 114.83(15) . 7_565 ?
O1 P1 O2 114.83(15) . . ?
O2 P1 O2 109.3(2) 7_565 . ?
O1 P1 C1 102.9(2) . . ?
O2 P1 C1 107.10(15) 7_565 . ?
O2 P1 C1 107.10(15) . . ?
C2 N1 C1 109.2(4) . . ?
C2 N1 H1B 109.8 . . ?
C1 N1 H1B 109.8 . . ?
N1 C1 P1 114.4(4) . . ?
N1 C1 H1A 108.4 . . ?
P1 C1 H1A 108.8 . . ?
N1 C2 C3 114.4(5) . . ?
N1 C2 H2A 108.5 . . ?
C3 C2 H2A 108.7 . . ?
C4 C3 C4 119.2(6) 7_565 . ?
C4 C3 C2 120.2(3) 7_565 . ?
C4 C3 C2 120.2(3) . . ?
C3 C4 C5 120.8(5) . . ?
C3 C4 H4A 119.3 . . ?
C5 C4 H4A 119.8 . . ?
C6 C5 C4 119.8(5) . . ?
C6 C5 H5A 119.4 . . ?
C4 C5 H5A 120.8 . . ?
C5 C6 C5 119.5(6) . 7_565 ?
C5 C6 C7 120.2(3) . . ?
C5 C6 C7 120.2(3) 7_565 . ?
O3 C7 O3 121.5(5) . 7_565 ?
O3 C7 C6 119.2(2) . . ?
O3 C7 C6 119.2(2) 7_565 . ?
O3 C7 Eu1 60.9(2) . 6_558 ?
O3 C7 Eu1 60.9(2) 7_565 6_558 ?
C6 C7 Eu1 174.8(4) . 6_558 ?
P1 O1 Eu1 162.5(3) . . ?
P1 O2 Eu1 148.47(19) . 2 ?
C7 O3 Eu1 93.3(3) . 6_558 ?
Eu1 O1W H1WA 109.3 . . ?
Eu1 O2W H2WA 109.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.247(4) . ?
Eu1 O2 2.252(3) 2_554 ?
Eu1 O2 2.252(3) 8_665 ?
Eu1 O1W 2.528(4) . ?
Eu1 O2W 2.539(4) . ?
Eu1 O3 2.540(3) 6_658 ?
Eu1 O3 2.540(3) 4_557 ?
Eu1 Cl1 2.8546(17) . ?
Eu1 C7 2.903(5) 6_658 ?
P1 O1 1.496(4) . ?
P1 O2 1.503(3) 7_565 ?
P1 O2 1.503(3) . ?
P1 C1 1.810(6) . ?
N1 C2 1.490(7) . ?
N1 C1 1.493(6) . ?
N1 H1B 0.9001 . ?
C1 H1A 0.9600 . ?
C2 C3 1.525(8) . ?
C2 H2A 0.9600 . ?
C3 C4 1.374(6) 7_565 ?
C3 C4 1.374(6) . ?
C4 C5 1.394(6) . ?
C4 H4A 0.9599 . ?
C5 C6 1.384(6) . ?
C5 H5A 0.9599 . ?
C6 C5 1.384(6) 7_565 ?
C6 C7 1.499(8) . ?
C7 O3 1.269(4) . ?
C7 O3 1.269(4) 7_565 ?
C7 Eu1 2.903(5) 6_558 ?
O2 Eu1 2.252(3) 2 ?
O3 Eu1 2.540(3) 6_558 ?
O1W H1WA 0.8500 . ?
O2W H2WA 0.8501 . ?
