#------------------------------------------------------------------------------
#$Date: 2018-09-27 07:13:35 +0300 (Thu, 27 Sep 2018) $
#$Revision: 211196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/14/4311483.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_4311483
loop_
_publ_author_name
'Jun-Ling Song'
'Chong Lei'
'Jiang-Gao Mao'
_publ_contact_author_address
;
     Fujian Institute of Research  
        on the Structure of Matter,
        Chinese Academy of Sciences,
        Fuzhou, Fujian 350002, 
    P.R.China
;
_publ_contact_author_email       mjg@ms.fjirsm.ac.cn
_publ_contact_author_fax         0086-0591-3714946
_publ_contact_author_name        'Dr. Jiang-Gao Mao'
_publ_contact_author_phone       0086-0591-3704836
_publ_section_title
;
 Syntheses, Crystal Structures, and Luminescent Properties of Novel
 Layered Lanthanide Sulfonate-Phosphonates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5630
_journal_page_last               5634
_journal_paper_doi               10.1021/ic049376u
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C12 H19 Gd N O15 P S'
_chemical_formula_sum            'C12 H19 Gd N O15 P S'
_chemical_formula_weight         637.56
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.2740(10)
_cell_angle_beta                 81.3400(10)
_cell_angle_gamma                77.8140(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6465(3)
_cell_length_b                   11.3948(3)
_cell_length_c                   11.9596(3)
_cell_measurement_temperature    293(2)
_cell_volume                     970.97(5)
_computing_cell_refinement       'Smart CCD Software(Siemens, 1994)'
_computing_data_collection       'Smart CCD Software(Siemens, 1994)'
_computing_data_reduction        'Smart CCD Software(Siemens, 1994)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Smart CCD'
_diffrn_measurement_method       'ω scan'
_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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5040
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0.9
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.687
_exptl_absorpt_correction_T_max  0.4807
_exptl_absorpt_correction_T_min  0.2980
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.709
_refine_diff_density_min         -1.545
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0583P)²+7.4281P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                3226
_reflns_number_total             3385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049376usi20040513_120609.cif
_cod_data_source_block           1
_cod_database_code               4311483
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.55448(4) 0.29933(3) 0.56524(2) 0.01749(14) Uani 1 1 d . . .
P1 P -0.4216(2) 0.51400(14) 0.72434(13) 0.0163(3) Uani 1 1 d . . .
S1 S 0.0930(2) -0.07731(14) 1.26332(13) 0.0192(3) Uani 1 1 d . . .
N1 N -0.0914(7) 0.5867(5) 0.7278(5) 0.0207(11) Uani 1 1 d . . .
H01A H -0.1324 0.6534 0.6690 0.025 Uiso 1 1 calc R . .
C1 C -0.2488(9) 0.5399(6) 0.8018(5) 0.0212(13) Uani 1 1 d . . .
H1A H -0.3052 0.5989 0.8467 0.025 Uiso 1 1 calc R . .
H1B H -0.2057 0.4620 0.8573 0.025 Uiso 1 1 calc R . .
C2 C 0.0275(9) 0.4899(6) 0.6730(6) 0.0252(14) Uani 1 1 d . . .
H2A H -0.0452 0.4576 0.6329 0.030 Uiso 1 1 calc R . .
H2B H 0.0809 0.4212 0.7342 0.030 Uiso 1 1 calc R . .
C3 C 0.1751(9) 0.5435(6) 0.5864(5) 0.0195(13) Uani 1 1 d . . .
C4 C 0.0135(10) 0.6298(8) 0.8006(7) 0.0325(17) Uani 1 1 d . . .
H4A H -0.0646 0.6900 0.8357 0.049 Uiso 1 1 calc R . .
H4B H 0.1095 0.6670 0.7515 0.049 Uiso 1 1 calc R . .
H4C H 0.0626 0.5599 0.8610 0.049 Uiso 1 1 calc R . .
C11 C 0.1825(9) -0.0451(6) 1.1139(5) 0.0193(13) Uani 1 1 d . . .
C12 C 0.2246(9) -0.1417(6) 1.0597(6) 0.0227(14) Uani 1 1 d . . .
H12A H 0.2003 -0.2203 1.0999 0.027 Uiso 1 1 calc R . .
C13 C 0.3035(9) -0.1195(6) 0.9446(6) 0.0217(13) Uani 1 1 d . . .
C14 C 0.3360(9) -0.0005(6) 0.8842(6) 0.0234(14) Uani 1 1 d . . .
H14A H 0.3864 0.0146 0.8068 0.028 Uiso 1 1 calc R . .
C15 C 0.2941(9) 0.0954(6) 0.9386(6) 0.0208(13) Uani 1 1 d . . .
C16 C 0.2169(9) 0.0733(6) 1.0540(6) 0.0224(13) Uani 1 1 d . . .
H16A H 0.1883 0.1373 1.0910 0.027 Uiso 1 1 calc R . .
C17 C 0.3598(9) -0.2185(6) 0.8821(6) 0.0244(14) Uani 1 1 d . . .
C18 C 0.3366(9) 0.2194(6) 0.8688(6) 0.0217(13) Uani 1 1 d . . .
O1 O 0.1521(7) 0.6577(5) 0.5400(4) 0.0324(12) Uani 1 1 d . . .
O2 O 0.3165(7) 0.4707(5) 0.5680(4) 0.0312(11) Uani 1 1 d . . .
O3 O 0.4498(9) -0.2023(5) 0.7872(5) 0.0418(14) Uani 1 1 d . . .
O4 O 0.3066(7) -0.3262(4) 0.9370(4) 0.0309(11) Uani 1 1 d . . .
H4D H 0.3470 -0.3769 0.8986 0.046 Uiso 1 1 calc R . .
O5 O 0.3120(8) 0.3038(5) 0.9284(4) 0.0329(12) Uani 1 1 d . . .
O6 O 0.3876(7) 0.2397(5) 0.7656(4) 0.0291(11) Uani 1 1 d . . .
O7 O -0.0047(7) 0.0397(5) 1.2837(5) 0.0339(12) Uani 1 1 d . . .
O8 O 0.2522(6) -0.1222(5) 1.3290(4) 0.0260(10) Uani 1 1 d . . .
O9 O -0.0145(7) -0.1726(5) 1.2803(4) 0.0302(11) Uani 1 1 d . . .
O11 O -0.5791(6) 0.5029(4) 0.8221(4) 0.0210(9) Uani 1 1 d . . .
H11A H -0.5940 0.4303 0.8454 0.031 Uiso 1 1 calc R . .
O12 O -0.3499(6) 0.3946(4) 0.6882(4) 0.0221(9) Uani 1 1 d . . .
O13 O -0.4577(7) 0.6285(4) 0.6245(4) 0.0250(10) Uani 1 1 d . . .
O1W O 0.3282(8) 0.1778(6) 0.5755(5) 0.0448(15) Uani 1 1 d . . .
O2W O 0.6716(9) 0.1426(5) 0.4446(5) 0.0418(14) Uani 1 1 d . . .
O3W O 0.2397(10) 0.1524(6) 0.3683(6) 0.0522(16) Uani 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O12 Gd1 O13 133.74(16) 1_655 2_566 ?
O12 Gd1 O2 77.96(16) 1_655 . ?
O13 Gd1 O2 73.31(16) 2_566 . ?
O12 Gd1 O8 81.89(16) 1_655 2_657 ?
O13 Gd1 O8 136.56(16) 2_566 2_657 ?
O2 Gd1 O8 148.87(16) . 2_657 ?
O12 Gd1 O1W 137.16(18) 1_655 . ?
O13 Gd1 O1W 76.84(19) 2_566 . ?
O2 Gd1 O1W 87.2(2) . . ?
O8 Gd1 O1W 91.8(2) 2_657 . ?
O12 Gd1 O1 79.18(17) 1_655 2_666 ?
O13 Gd1 O1 83.42(18) 2_566 2_666 ?
O2 Gd1 O1 118.23(18) . 2_666 ?
O8 Gd1 O1 80.33(17) 2_657 2_666 ?
O1W Gd1 O1 141.65(19) . 2_666 ?
O12 Gd1 O6 71.18(16) 1_655 . ?
O13 Gd1 O6 132.26(18) 2_566 . ?
O2 Gd1 O6 75.61(18) . . ?
O8 Gd1 O6 75.55(17) 2_657 . ?
O1W Gd1 O6 66.23(17) . . ?
O1 Gd1 O6 143.88(18) 2_666 . ?
O12 Gd1 O2W 141.28(18) 1_655 . ?
O13 Gd1 O2W 67.90(17) 2_566 . ?
O2 Gd1 O2W 138.55(18) . . ?
O8 Gd1 O2W 68.77(17) 2_657 . ?
O1W Gd1 O2W 70.5(2) . . ?
O1 Gd1 O2W 71.6(2) 2_666 . ?
O6 Gd1 O2W 121.83(18) . . ?
O12 Gd1 O2 68.51(15) 1_655 2_666 ?
O13 Gd1 O2 68.29(15) 2_566 2_666 ?
O2 Gd1 O2 71.24(18) . 2_666 ?
O8 Gd1 O2 122.28(15) 2_657 2_666 ?
O1W Gd1 O2 142.86(18) . 2_666 ?
O1 Gd1 O2 47.00(15) 2_666 2_666 ?
O6 Gd1 O2 131.85(15) . 2_666 ?
O2W Gd1 O2 106.10(17) . 2_666 ?
O12 Gd1 C3 73.81(16) 1_655 2_666 ?
O13 Gd1 C3 73.58(17) 2_566 2_666 ?
O2 Gd1 C3 95.19(18) . 2_666 ?
O8 Gd1 C3 101.70(17) 2_657 2_666 ?
O1W Gd1 C3 148.22(18) . 2_666 ?
O1 Gd1 C3 23.09(17) 2_666 2_666 ?
O6 Gd1 C3 144.92(16) . 2_666 ?
O2W Gd1 C3 87.60(19) . 2_666 ?
O2 Gd1 C3 23.97(16) 2_666 2_666 ?
O13 P1 O12 114.9(3) . . ?
O13 P1 O11 112.9(3) . . ?
O12 P1 O11 113.4(3) . . ?
O13 P1 C1 106.1(3) . . ?
O12 P1 C1 107.4(3) . . ?
O11 P1 C1 100.7(3) . . ?
O9 S1 O7 115.2(3) . . ?
O9 S1 O8 112.5(3) . . ?
O7 S1 O8 110.8(3) . . ?
O9 S1 C11 106.3(3) . . ?
O7 S1 C11 107.1(3) . . ?
O8 S1 C11 104.2(3) . . ?
C1 N1 C4 109.1(5) . . ?
C1 N1 C2 112.3(5) . . ?
C4 N1 C2 110.7(5) . . ?
N1 C1 P1 116.4(4) . . ?
N1 C2 C3 111.7(5) . . ?
O1 C3 O2 123.4(6) . . ?
O1 C3 C2 118.7(6) . . ?
O2 C3 C2 117.9(6) . . ?
O1 C3 Gd1 51.2(3) . 2_666 ?
O2 C3 Gd1 72.5(4) . 2_666 ?
C2 C3 Gd1 167.4(4) . 2_666 ?
C12 C11 C16 120.7(6) . . ?
C12 C11 S1 118.7(5) . . ?
C16 C11 S1 120.5(5) . . ?
C11 C12 C13 119.4(6) . . ?
C12 C13 C14 119.8(6) . . ?
C12 C13 C17 122.8(6) . . ?
C14 C13 C17 117.4(6) . . ?
C15 C14 C13 120.7(6) . . ?
C14 C15 C16 119.7(6) . . ?
C14 C15 C18 117.4(6) . . ?
C16 C15 C18 123.0(6) . . ?
C15 C16 C11 119.8(6) . . ?
O3 C17 O4 122.4(6) . . ?
O3 C17 C13 122.3(6) . . ?
O4 C17 C13 115.3(6) . . ?
O6 C18 O5 123.4(6) . . ?
O6 C18 C15 121.7(6) . . ?
O5 C18 C15 114.9(6) . . ?
C3 O1 Gd1 105.7(4) . 2_666 ?
C3 O2 Gd1 167.4(5) . . ?
C3 O2 Gd1 83.5(4) . 2_666 ?
Gd1 O2 Gd1 108.76(18) . 2_666 ?
C18 O6 Gd1 166.1(5) . . ?
S1 O8 Gd1 146.3(3) . 2_657 ?
P1 O12 Gd1 133.5(3) . 1_455 ?
P1 O13 Gd1 143.1(3) . 2_566 ?
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 O12 2.335(4) 1_655 ?
Gd1 O13 2.356(4) 2_566 ?
Gd1 O2 2.376(5) . ?
Gd1 O8 2.386(5) 2_657 ?
Gd1 O1W 2.404(5) . ?
Gd1 O1 2.473(5) 2_666 ?
Gd1 O6 2.518(5) . ?
Gd1 O2W 2.548(5) . ?
Gd1 O2 2.932(6) 2_666 ?
Gd1 C3 3.055(6) 2_666 ?
P1 O13 1.501(5) . ?
P1 O12 1.514(5) . ?
P1 O11 1.545(4) . ?
P1 C1 1.839(7) . ?
S1 O9 1.448(5) . ?
S1 O7 1.452(5) . ?
S1 O8 1.468(5) . ?
S1 C11 1.776(7) . ?
N1 C1 1.481(8) . ?
N1 C4 1.506(8) . ?
N1 C2 1.512(8) . ?
C2 C3 1.515(9) . ?
C3 O1 1.245(8) . ?
C3 O2 1.249(8) . ?
C3 Gd1 3.055(6) 2_666 ?
C11 C12 1.391(9) . ?
C11 C16 1.392(9) . ?
C12 C13 1.392(9) . ?
C13 C14 1.396(9) . ?
C13 C17 1.483(9) . ?
C14 C15 1.385(10) . ?
C15 C16 1.391(9) . ?
C15 C18 1.493(9) . ?
C17 O3 1.222(9) . ?
C17 O4 1.330(8) . ?
C18 O6 1.208(8) . ?
C18 O5 1.321(9) . ?
O1 Gd1 2.473(5) 2_666 ?
O2 Gd1 2.932(6) 2_666 ?
O8 Gd1 2.386(5) 2_657 ?
O12 Gd1 2.335(4) 1_455 ?
O13 Gd1 2.356(4) 2_566 ?
