#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:59:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179224 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/46/4314634.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_4314634
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 Gd N O7 P'
_chemical_formula_sum            'C9 H14 Cl Gd N O7 P'
_chemical_formula_weight         471.88
_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                   23.515(12)
_cell_length_b                   6.828(3)
_cell_length_c                   8.743(4)
_cell_measurement_reflns_used    1671
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4603
_cell_measurement_theta_min      2.4865
_cell_volume                     1403.8(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0198
_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       -10
_diffrn_reflns_number            10359
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    5.057
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4983
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0194P)²+2.3008P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0468
_reflns_number_gt                1632
_reflns_number_total             1727
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901621x_si_001_3.cif
_cod_data_source_block           3
_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_original_cell_volume        1403.8(12)
_cod_database_code               4314634
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
Gd1 Gd 0.291307(8) 0.2500 0.65809(2) 0.01447(8) Uani 1 2 d S . .
Cl1 Cl 0.40748(5) 0.2500 0.56644(16) 0.0501(4) Uani 1 2 d S . .
P1 P 0.20967(4) 0.2500 1.01971(11) 0.0150(2) Uani 1 2 d S . .
N1 N 0.09947(14) 0.2500 1.1370(4) 0.0240(8) Uani 1 2 d S . .
H1B H 0.1079 0.3570 1.1927 0.029 Uiso 1 1 d R . .
C1 C 0.13329(18) 0.2500 0.9904(5) 0.0289(10) Uani 1 2 d S . .
H1A H 0.1230 0.1364 0.9319 0.035 Uiso 1 1 d R . .
C2 C 0.03738(19) 0.2500 1.0997(6) 0.0455(15) Uani 1 2 d S . .
H2A H 0.0294 0.1364 1.0386 0.055 Uiso 1 1 d R . .
C3 C -0.00203(19) 0.2500 1.2360(5) 0.0365(12) Uani 1 2 d S . .
C4 C -0.02249(15) 0.4248(7) 1.2939(4) 0.0430(9) Uani 1 1 d . . .
H4A H -0.0075 0.5462 1.2558 0.052 Uiso 1 1 d R . .
C5 C -0.06435(15) 0.4249(6) 1.4070(4) 0.0400(8) Uani 1 1 d . . .
H5A H -0.0789 0.5462 1.4466 0.048 Uiso 1 1 d R . .
C6 C -0.08598(18) 0.2500 1.4629(5) 0.0291(10) Uani 1 2 d S . .
C7 C -0.13108(19) 0.2500 1.5845(5) 0.0274(10) Uani 1 2 d S . .
O1 O 0.23267(14) 0.2500 0.8597(3) 0.0342(8) Uani 1 2 d S . .
O2 O 0.22392(10) 0.0698(3) 1.1120(3) 0.0311(5) Uani 1 1 d . . .
O3 O -0.14884(9) 0.4121(3) 1.6364(2) 0.0320(5) Uani 1 1 d . . .
O1W O 0.19423(15) 0.2500 0.5362(4) 0.0380(8) Uani 1 2 d S . .
H1WA H 0.1906 0.3516 0.4808 0.057 Uiso 1 1 d R . .
O2W O 0.29899(17) 0.2500 0.3687(4) 0.0473(10) Uani 1 2 d S . .
H2WA H 0.3170 0.3516 0.3402 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'
Gd Gd -0.1653 3.9035 '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 Gd1 O2 92.46(6) . 2_554 ?
O1 Gd1 O2 92.46(6) . 8_665 ?
O2 Gd1 O2 152.27(13) 2_554 8_665 ?
O1 Gd1 O1W 76.99(12) . . ?
O2 Gd1 O1W 77.29(6) 2_554 . ?
O2 Gd1 O1W 77.29(6) 8_665 . ?
O1 Gd1 O2W 146.04(12) . . ?
O2 Gd1 O2W 80.37(6) 2_554 . ?
O2 Gd1 O2W 80.37(6) 8_665 . ?
O1W Gd1 O2W 69.05(12) . . ?
O1 Gd1 O3 77.53(10) . 6_658 ?
O2 Gd1 O3 129.71(8) 2_554 6_658 ?
O2 Gd1 O3 77.97(9) 8_665 6_658 ?
O1W Gd1 O3 143.36(8) . 6_658 ?
O2W Gd1 O3 131.84(9) . 6_658 ?
O1 Gd1 O3 77.53(10) . 4_557 ?
O2 Gd1 O3 77.97(8) 2_554 4_557 ?
O2 Gd1 O3 129.71(8) 8_665 4_557 ?
O1W Gd1 O3 143.36(8) . 4_557 ?
O2W Gd1 O3 131.84(9) . 4_557 ?
O3 Gd1 O3 51.74(11) 6_658 4_557 ?
O1 Gd1 Cl1 144.39(9) . . ?
O2 Gd1 Cl1 95.87(6) 2_554 . ?
O2 Gd1 Cl1 95.87(6) 8_665 . ?
O1W Gd1 Cl1 138.62(10) . . ?
O2W Gd1 Cl1 69.57(9) . . ?
O3 Gd1 Cl1 70.55(6) 6_658 . ?
O3 Gd1 Cl1 70.55(6) 4_557 . ?
O1 Gd1 C7 77.09(13) . 6_658 ?
O2 Gd1 C7 103.85(6) 2_554 6_658 ?
O2 Gd1 C7 103.85(6) 8_665 6_658 ?
O1W Gd1 C7 154.07(12) . 6_658 ?
O2W Gd1 C7 136.87(13) . 6_658 ?
O3 Gd1 C7 25.89(5) 6_658 6_658 ?
O3 Gd1 C7 25.89(5) 4_557 6_658 ?
Cl1 Gd1 C7 67.30(9) . 6_658 ?
O1 P1 O2 114.75(12) . 7_565 ?
O1 P1 O2 114.75(12) . . ?
O2 P1 O2 109.24(19) 7_565 . ?
O1 P1 C1 103.02(19) . . ?
O2 P1 C1 107.17(12) 7_565 . ?
O2 P1 C1 107.17(12) . . ?
C2 N1 C1 109.2(3) . . ?
C2 N1 H1B 109.5 . . ?
C1 N1 H1B 110.1 . . ?
N1 C1 P1 113.7(3) . . ?
N1 C1 H1A 108.7 . . ?
P1 C1 H1A 108.9 . . ?
N1 C2 C3 115.3(4) . . ?
N1 C2 H2A 108.2 . . ?
C3 C2 H2A 108.5 . . ?
C4 C3 C4 119.3(4) . 7_565 ?
C4 C3 C2 120.2(2) . . ?
C4 C3 C2 120.2(2) 7_565 . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4A 119.4 . . ?
C5 C4 H4A 120.3 . . ?
C6 C5 C4 120.5(4) . . ?
C6 C5 H5A 119.0 . . ?
C4 C5 H5A 120.4 . . ?
C5 C6 C5 118.9(4) 7_565 . ?
C5 C6 C7 120.6(2) 7_565 . ?
C5 C6 C7 120.6(2) . . ?
O3 C7 O3 121.8(4) . 7_565 ?
O3 C7 C6 119.09(19) . . ?
O3 C7 C6 119.09(19) 7_565 . ?
O3 C7 Gd1 60.94(19) . 6_558 ?
O3 C7 Gd1 60.94(19) 7_565 6_558 ?
C6 C7 Gd1 174.1(3) . 6_558 ?
P1 O1 Gd1 163.1(2) . . ?
P1 O2 Gd1 148.43(15) . 2 ?
C7 O3 Gd1 93.2(2) . 6_558 ?
Gd1 O1W H1WA 109.3 . . ?
Gd1 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
Gd1 O1 2.238(3) . ?
Gd1 O2 2.249(2) 2_554 ?
Gd1 O2 2.249(2) 8_665 ?
Gd1 O1W 2.519(3) . ?
Gd1 O2W 2.537(4) . ?
Gd1 O3 2.537(2) 6_658 ?
Gd1 O3 2.537(2) 4_557 ?
Gd1 Cl1 2.8470(18) . ?
Gd1 C7 2.897(4) 6_658 ?
P1 O1 1.500(3) . ?
P1 O2 1.509(2) 7_565 ?
P1 O2 1.509(2) . ?
P1 C1 1.814(4) . ?
N1 C2 1.496(5) . ?
N1 C1 1.508(5) . ?
N1 H1B 0.9005 . ?
C1 H1A 0.9604 . ?
C2 C3 1.510(6) . ?
C2 H2A 0.9603 . ?
C3 C4 1.383(5) . ?
C3 C4 1.383(5) 7_565 ?
C4 C5 1.396(5) . ?
C4 H4A 0.9602 . ?
C5 C6 1.387(4) . ?
C5 H5A 0.9602 . ?
C6 C5 1.387(4) 7_565 ?
C6 C7 1.502(6) . ?
C7 O3 1.267(3) . ?
C7 O3 1.267(3) 7_565 ?
C7 Gd1 2.897(4) 6_558 ?
O2 Gd1 2.249(2) 2 ?
O3 Gd1 2.537(2) 6_558 ?
O1W H1WA 0.8503 . ?
O2W H2WA 0.8503 . ?
