#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:59:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179224 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/46/4314632.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_4314632
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 N O7 P Sm'
_chemical_formula_sum            'C9 H14 Cl N O7 P Sm'
_chemical_formula_weight         464.98
_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                   23.5128(19)
_cell_length_b                   6.8407(5)
_cell_length_c                   8.7416(8)
_cell_measurement_reflns_used    3836
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1009
_cell_volume                     1406.0(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 14.6306
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Mercury70 (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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       30
_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            10397
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    4.508
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5296
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.783
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0268
_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)+(0.0265P)²+4.7373P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                1681
_reflns_number_total             1746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901621x_si_001_1.cif
_cod_data_source_block           1
_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               4314632
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
Sm1 Sm 0.291284(9) 0.2500 0.65874(3) 0.01484(9) Uani 1 2 d S . .
Cl1 Cl 0.40812(7) 0.2500 0.5682(2) 0.0755(8) Uani 1 2 d S . .
P1 P 0.20925(5) 0.2500 1.02081(14) 0.0155(2) Uani 1 2 d S . .
N1 N 0.09927(17) 0.2500 1.1369(5) 0.0263(10) Uani 1 2 d S . .
H1B H 0.1077 0.3570 1.1926 0.032 Uiso 1 1 d R . .
C1 C 0.1327(2) 0.2500 0.9909(6) 0.0370(15) Uani 1 2 d S . .
H1A H 0.1224 0.1364 0.9323 0.044 Uiso 1 1 d R . .
C2 C 0.0375(2) 0.2500 1.0993(7) 0.075(3) Uani 1 2 d S . .
H2A H 0.0294 0.1364 1.0382 0.091 Uiso 1 1 d R . .
C3 C -0.0022(2) 0.2500 1.2358(7) 0.057(2) Uani 1 2 d S . .
C4 C -0.02239(19) 0.4236(11) 1.2937(5) 0.0603(17) Uani 1 1 d . . .
H4A H -0.0074 0.5450 1.2557 0.072 Uiso 1 1 d R . .
C5 C -0.06421(19) 0.4247(9) 1.4065(5) 0.0504(13) Uani 1 1 d . . .
H5A H -0.0787 0.5460 1.4460 0.060 Uiso 1 1 d R . .
C6 C -0.0853(2) 0.2500 1.4621(6) 0.0383(15) Uani 1 2 d S . .
C7 C -0.1305(2) 0.2500 1.5828(6) 0.0314(13) Uani 1 2 d S . .
O1 O 0.23183(17) 0.2500 0.8613(4) 0.0359(10) Uani 1 2 d S . .
O2 O 0.22367(13) 0.0714(4) 1.1128(4) 0.0357(7) Uani 1 1 d . . .
O3 O -0.14856(11) 0.4117(5) 1.6348(3) 0.0367(7) Uani 1 1 d . . .
O1W O 0.19390(18) 0.2500 0.5341(5) 0.0408(10) Uani 1 2 d S . .
H1WA H 0.1903 0.3516 0.4787 0.061 Uiso 1 1 d R . .
O2W O 0.2997(2) 0.2500 0.3678(5) 0.0474(12) Uani 1 2 d S . .
H2WA H 0.3177 0.3516 0.3393 0.071 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'
Sm Sm -0.1638 3.4418 '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 Sm1 O2 92.47(8) . 2_554 ?
O1 Sm1 O2 92.47(8) . 8_665 ?
O2 Sm1 O2 152.71(17) 2_554 8_665 ?
O1 Sm1 O1W 77.16(15) . . ?
O2 Sm1 O1W 77.49(8) 2_554 . ?
O2 Sm1 O1W 77.49(8) 8_665 . ?
O1 Sm1 O3 77.75(11) . 6_658 ?
O2 Sm1 O3 129.38(11) 2_554 6_658 ?
O2 Sm1 O3 77.87(11) 8_665 6_658 ?
O1W Sm1 O3 143.74(10) . 6_658 ?
O1 Sm1 O3 77.75(11) . 4_557 ?
O2 Sm1 O3 77.87(11) 2_554 4_557 ?
O2 Sm1 O3 129.38(11) 8_665 4_557 ?
O1W Sm1 O3 143.74(10) . 4_557 ?
O3 Sm1 O3 51.51(14) 6_658 4_557 ?
O1 Sm1 O2W 146.15(15) . . ?
O2 Sm1 O2W 80.50(8) 2_554 . ?
O2 Sm1 O2W 80.50(8) 8_665 . ?
O1W Sm1 O2W 68.99(15) . . ?
O3 Sm1 O2W 131.59(11) 6_658 . ?
O3 Sm1 O2W 131.59(11) 4_557 . ?
O1 Sm1 Cl1 144.37(11) . . ?
O2 Sm1 Cl1 95.75(8) 2_554 . ?
O2 Sm1 Cl1 95.75(8) 8_665 . ?
O1W Sm1 Cl1 138.47(12) . . ?
O3 Sm1 Cl1 70.28(7) 6_658 . ?
O3 Sm1 Cl1 70.28(7) 4_557 . ?
O2W Sm1 Cl1 69.48(11) . . ?
O1 Sm1 C7 77.43(14) . 6_658 ?
O2 Sm1 C7 103.64(8) 2_554 6_658 ?
O2 Sm1 C7 103.64(8) 8_665 6_658 ?
O1W Sm1 C7 154.60(15) . 6_658 ?
O3 Sm1 C7 25.78(7) 6_658 6_658 ?
O3 Sm1 C7 25.78(7) 4_557 6_658 ?
O2W Sm1 C7 136.41(15) . 6_658 ?
Cl1 Sm1 C7 66.93(11) . 6_658 ?
O1 P1 O2 114.85(15) . 7_565 ?
O1 P1 O2 114.85(15) . . ?
O2 P1 O2 108.9(2) 7_565 . ?
O1 P1 C1 102.6(2) . . ?
O2 P1 C1 107.48(15) 7_565 . ?
O2 P1 C1 107.48(15) . . ?
C2 N1 C1 108.8(4) . . ?
C2 N1 H1B 109.6 . . ?
C1 N1 H1B 110.1 . . ?
N1 C1 P1 113.3(4) . . ?
N1 C1 H1A 108.8 . . ?
P1 C1 H1A 109.0 . . ?
N1 C2 C3 115.2(5) . . ?
N1 C2 H2A 108.3 . . ?
C3 C2 H2A 108.4 . . ?
C4 C3 C4 119.5(6) 7_565 . ?
C4 C3 C2 120.1(3) 7_565 . ?
C4 C3 C2 120.1(3) . . ?
C3 C4 C5 120.5(6) . . ?
C3 C4 H4A 119.5 . . ?
C5 C4 H4A 120.0 . . ?
C6 C5 C4 119.8(6) . . ?
C6 C5 H5A 119.5 . . ?
C4 C5 H5A 120.6 . . ?
C5 C6 C5 119.7(6) . 7_565 ?
C5 C6 C7 120.1(3) . . ?
C5 C6 C7 120.1(3) 7_565 . ?
O3 C7 O3 121.3(5) 7_565 . ?
O3 C7 C6 119.3(2) 7_565 . ?
O3 C7 C6 119.3(2) . . ?
O3 C7 Sm1 60.7(2) 7_565 6_558 ?
O3 C7 Sm1 60.7(2) . 6_558 ?
C6 C7 Sm1 173.9(4) . 6_558 ?
P1 O1 Sm1 162.6(3) . . ?
P1 O2 Sm1 148.29(18) . 2 ?
C7 O3 Sm1 93.5(2) . 6_558 ?
Sm1 O1W H1WA 109.5 . . ?
Sm1 O2W H2WA 109.3 . . ?
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
Sm1 O1 2.256(3) . ?
Sm1 O2 2.263(3) 2_554 ?
Sm1 O2 2.263(3) 8_665 ?
Sm1 O1W 2.536(4) . ?
Sm1 O3 2.546(3) 6_658 ?
Sm1 O3 2.546(3) 4_557 ?
Sm1 O2W 2.551(4) . ?
Sm1 Cl1 2.8590(15) . ?
Sm1 C7 2.913(5) 6_658 ?
P1 O1 1.492(4) . ?
P1 O2 1.501(3) 7_565 ?
P1 O2 1.501(3) . ?
P1 C1 1.819(5) . ?
N1 C2 1.490(7) . ?
N1 C1 1.499(6) . ?
N1 H1B 0.9015 . ?
C1 H1A 0.9615 . ?
C2 C3 1.515(8) . ?
C2 H2A 0.9615 . ?
C3 C4 1.375(7) 7_565 ?
C3 C4 1.375(7) . ?
C4 C5 1.392(6) . ?
C4 H4A 0.9615 . ?
C5 C6 1.382(6) . ?
C5 H5A 0.9615 . ?
C6 C5 1.382(6) 7_565 ?
C6 C7 1.498(7) . ?
C7 O3 1.269(4) 7_565 ?
C7 O3 1.269(4) . ?
C7 Sm1 2.913(5) 6_558 ?
O2 Sm1 2.263(3) 2 ?
O3 Sm1 2.546(3) 6_558 ?
O1W H1WA 0.8513 . ?
O2W H2WA 0.8514 . ?
