#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:59:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179224 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/46/4314635.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_4314635
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 Tb'
_chemical_formula_sum            'C9 H14 Cl N O7 P Tb'
_chemical_formula_weight         473.55
_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                   23.480(3)
_cell_length_b                   6.7749(7)
_cell_length_c                   8.6854(9)
_cell_measurement_reflns_used    4019
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0066
_cell_volume                     1381.6(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0206
_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            9655
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    5.457
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5341
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.472
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0197
_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)+(0.0167P)²+2.2974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0450
_reflns_number_gt                1663
_reflns_number_total             1713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901621x_si_001_4.cif
_cod_data_source_block           4
_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               4314635
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
Tb1 Tb 0.291090(7) 0.2500 0.658907(18) 0.01320(6) Uani 1 2 d S . .
Cl1 Cl 0.40692(5) 0.2500 0.56649(14) 0.0458(3) Uani 1 2 d S . .
P1 P 0.20974(4) 0.2500 1.02053(11) 0.01331(18) Uani 1 2 d S . .
N1 N 0.09954(13) 0.2500 1.1372(4) 0.0217(7) Uani 1 2 d S . .
H1B H 0.1080 0.3570 1.1929 0.026 Uiso 1 1 d R . .
C1 C 0.13339(16) 0.2500 0.9904(4) 0.0254(9) Uani 1 2 d S . .
H1A H 0.1231 0.1364 0.9318 0.030 Uiso 1 1 d R . .
C2 C 0.03758(17) 0.2500 1.0991(5) 0.0406(13) Uani 1 2 d S . .
H2A H 0.0296 0.1364 1.0381 0.049 Uiso 1 1 d R . .
C3 C -0.00214(17) 0.2500 1.2359(5) 0.0330(11) Uani 1 2 d S . .
C4 C -0.02265(14) 0.4256(6) 1.2937(4) 0.0406(8) Uani 1 1 d . . .
H4A H -0.0077 0.5470 1.2556 0.049 Uiso 1 1 d R . .
C5 C -0.06465(14) 0.4256(5) 1.4066(4) 0.0375(8) Uani 1 1 d . . .
H5A H -0.0792 0.5469 1.4461 0.045 Uiso 1 1 d R . .
C6 C -0.08606(17) 0.2500 1.4622(5) 0.0294(9) Uani 1 2 d S . .
C7 C -0.13094(17) 0.2500 1.5844(4) 0.0260(9) Uani 1 2 d S . .
O1 O 0.23291(13) 0.2500 0.8602(3) 0.0332(7) Uani 1 2 d S . .
O2 O 0.22398(9) 0.0691(3) 1.1135(2) 0.0284(4) Uani 1 1 d . . .
O3 O -0.14924(9) 0.4136(3) 1.6364(2) 0.0303(5) Uani 1 1 d . . .
O1W O 0.19437(14) 0.2500 0.5385(4) 0.0370(8) Uani 1 2 d S . .
H1WA H 0.1908 0.3516 0.4832 0.055 Uiso 1 1 d R . .
O2W O 0.29855(15) 0.2500 0.3707(4) 0.0451(9) Uani 1 2 d S . .
H2WA H 0.3166 0.3516 0.3422 0.068 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'
Tb Tb -0.1723 4.1537 '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 Tb1 O2 92.39(6) . 2_554 ?
O1 Tb1 O2 92.39(6) . 8_665 ?
O2 Tb1 O2 152.46(11) 2_554 8_665 ?
O1 Tb1 O1W 76.73(11) . . ?
O2 Tb1 O1W 77.38(6) 2_554 . ?
O2 Tb1 O1W 77.38(6) 8_665 . ?
O1 Tb1 O2W 146.01(11) . . ?
O2 Tb1 O2W 80.47(6) 2_554 . ?
O2 Tb1 O2W 80.47(6) 8_665 . ?
O1W Tb1 O2W 69.28(12) . . ?
O1 Tb1 O3 77.67(9) . 6_658 ?
O2 Tb1 O3 129.82(8) 2_554 6_658 ?
O2 Tb1 O3 77.65(8) 8_665 6_658 ?
O1W Tb1 O3 143.13(7) . 6_658 ?
O2W Tb1 O3 131.67(8) . 6_658 ?
O1 Tb1 O3 77.67(9) . 4_557 ?
O2 Tb1 O3 77.65(8) 2_554 4_557 ?
O2 Tb1 O3 129.82(8) 8_665 4_557 ?
O1W Tb1 O3 143.13(7) . 4_557 ?
O2W Tb1 O3 131.67(8) . 4_557 ?
O3 Tb1 O3 52.18(10) 6_658 4_557 ?
O1 Tb1 Cl1 144.44(8) . . ?
O2 Tb1 Cl1 95.87(6) 2_554 . ?
O2 Tb1 Cl1 95.87(6) 8_665 . ?
O1W Tb1 Cl1 138.83(9) . . ?
O2W Tb1 Cl1 69.55(9) . . ?
O3 Tb1 Cl1 70.51(5) 6_658 . ?
O3 Tb1 Cl1 70.51(5) 4_557 . ?
O1 Tb1 C7 77.39(11) . 6_658 ?
O2 Tb1 C7 103.75(6) 2_554 6_658 ?
O2 Tb1 C7 103.75(6) 8_665 6_658 ?
O1W Tb1 C7 154.12(11) . 6_658 ?
O2W Tb1 C7 136.60(11) . 6_658 ?
O3 Tb1 C7 26.11(5) 6_658 6_658 ?
O3 Tb1 C7 26.11(5) 4_557 6_658 ?
Cl1 Tb1 C7 67.05(8) . 6_658 ?
O1 P1 O2 114.76(11) . 7_565 ?
O1 P1 O2 114.76(10) . . ?
O2 P1 O2 109.00(17) 7_565 . ?
O1 P1 C1 103.05(17) . . ?
O2 P1 C1 107.30(11) 7_565 . ?
O2 P1 C1 107.30(11) . . ?
C2 N1 C1 109.1(3) . . ?
C2 N1 H1B 109.7 . . ?
C1 N1 H1B 110.0 . . ?
N1 C1 P1 113.6(3) . . ?
N1 C1 H1A 108.6 . . ?
P1 C1 H1A 109.1 . . ?
N1 C2 C3 115.3(3) . . ?
N1 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
C4 C3 C4 119.4(4) . 7_565 ?
C4 C3 C2 120.2(2) . . ?
C4 C3 C2 120.15(19) 7_565 . ?
C3 C4 C5 120.3(3) . . ?
C3 C4 H4A 119.3 . . ?
C5 C4 H4A 120.4 . . ?
C6 C5 C4 120.4(3) . . ?
C6 C5 H5A 119.1 . . ?
C4 C5 H5A 120.5 . . ?
C5 C6 C5 119.3(4) . 7_565 ?
C5 C6 C7 120.36(19) . . ?
C5 C6 C7 120.36(19) 7_565 . ?
O3 C7 O3 121.3(4) . 7_565 ?
O3 C7 C6 119.35(18) . . ?
O3 C7 C6 119.35(18) 7_565 . ?
O3 C7 Tb1 60.73(18) . 6_558 ?
O3 C7 Tb1 60.73(17) 7_565 6_558 ?
C6 C7 Tb1 174.6(3) . 6_558 ?
P1 O1 Tb1 163.4(2) . . ?
P1 O2 Tb1 148.26(13) . 2 ?
C7 O3 Tb1 93.16(19) . 6_558 ?
Tb1 O1W H1WA 109.2 . . ?
Tb1 O2W H2WA 109.1 . . ?
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
Tb1 O1 2.219(3) . ?
Tb1 O2 2.2260(19) 2_554 ?
Tb1 O2 2.2260(19) 8_665 ?
Tb1 O1W 2.500(3) . ?
Tb1 O2W 2.509(3) . ?
Tb1 O3 2.520(2) 6_658 ?
Tb1 O3 2.5200(19) 4_557 ?
Tb1 Cl1 2.8356(12) . ?
Tb1 C7 2.885(4) 6_658 ?
P1 O1 1.495(3) . ?
P1 O2 1.505(2) 7_565 ?
P1 O2 1.505(2) . ?
P1 C1 1.812(4) . ?
N1 C2 1.492(5) . ?
N1 C1 1.502(4) . ?
N1 H1B 0.8941 . ?
C1 H1A 0.9535 . ?
C2 C3 1.510(5) . ?
C2 H2A 0.9534 . ?
C3 C4 1.378(4) . ?
C3 C4 1.378(4) 7_565 ?
C4 C5 1.390(4) . ?
C4 H4A 0.9536 . ?
C5 C6 1.379(4) . ?
C5 H5A 0.9537 . ?
C6 C5 1.379(4) 7_565 ?
C6 C7 1.496(5) . ?
C7 O3 1.271(3) . ?
C7 O3 1.271(3) 7_565 ?
C7 Tb1 2.885(4) 6_558 ?
O2 Tb1 2.2260(19) 2 ?
O3 Tb1 2.5200(19) 6_558 ?
O1W H1WA 0.8441 . ?
O2W H2WA 0.8451 . ?
