#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/11/4311166.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_4311166
loop_
_publ_author_name
'Subhadip Neogi'
'G. Savitha'
'Parimal K. Bharadwaj'
_publ_section_title
;
 Structure of Discrete (H2O)12 Clusters Present in the Cavity of Polymeric
 Interlinked Metallocycles of Nd(III) or Gd(III) and a Podand Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3771
_journal_page_last               3773
_journal_paper_doi               10.1021/ic0495618
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C28 H37 N Gd O17'
_chemical_formula_sum            'C28 H37 Gd N O17'
_chemical_formula_weight         816.84
_chemical_name_systematic
;
 ?
;
_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                95.385(5)
_cell_angle_beta                 103.105(5)
_cell_angle_gamma                108.467(5)
_cell_formula_units_Z            2
_cell_length_a                   10.861(5)
_cell_length_b                   11.600(5)
_cell_length_c                   13.806(5)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.04
_cell_volume                     1580.8(12)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 ( Bruker, 2003)'
_computing_publication_material  'Diamond 2.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10607
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    2.143
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular parallelopiped'
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0431P)²+2.1178P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                7214
_reflns_number_total             7523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0495618rom20040404_080710_2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1580.8(11)
_cod_original_formula_sum        'C28 H37 N Gd O17'
_cod_database_code               4311166
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 0.283290(12) 0.468727(11) 0.567516(8) 0.01378(5) Uani 1 1 d . . .
O1 O -0.2943(2) 0.06299(18) 1.06339(15) 0.0205(4) Uani 1 1 d . . .
O2 O -0.6312(2) -0.43803(17) 0.75167(14) 0.0178(4) Uani 1 1 d . . .
O3 O -0.5706(2) -0.31561(19) 0.64496(15) 0.0248(4) Uani 1 1 d . . .
O4 O 0.0547(2) 0.17413(19) 1.05522(15) 0.0219(4) Uani 1 1 d . . .
O5 O -0.1464(2) 0.35163(19) 1.01091(14) 0.0196(4) Uani 1 1 d . . .
O6 O -0.0225(3) 0.1488(2) 0.58421(16) 0.0310(5) Uani 1 1 d . . .
O7 O 0.1576(2) 0.3206(2) 0.64217(16) 0.0293(5) Uani 1 1 d . . .
O8 O 0.6680(2) 0.43817(19) 0.56658(14) 0.0200(4) Uani 1 1 d . . .
O9 O 0.4876(2) 0.4416(2) 0.61483(15) 0.0225(4) Uani 1 1 d . . .
O10 O 0.1440(2) 0.58719(18) 0.59626(14) 0.0191(4) Uani 1 1 d . . .
O11 O -0.06093(19) 0.60280(18) 0.55701(14) 0.0185(4) Uani 1 1 d . . .
N1 N -0.0773(2) 0.2481(2) 1.18083(16) 0.0155(4) Uani 1 1 d . . .
C1 C -0.1785(3) 0.1690(2) 1.2280(2) 0.0183(5) Uani 1 1 d . . .
H1A H -0.2460 0.2059 1.2328 0.022 Uiso 1 1 calc R . .
H1B H -0.1336 0.1632 1.2956 0.022 Uiso 1 1 calc R . .
C2 C -0.2455(3) 0.0412(3) 1.1633(2) 0.0195(5) Uani 1 1 d . . .
H2A H -0.1812 -0.0010 1.1644 0.023 Uiso 1 1 calc R . .
H2B H -0.3193 -0.0083 1.1869 0.023 Uiso 1 1 calc R . .
C3 C -0.3585(3) -0.0371(2) 0.9865(2) 0.0181(5) Uani 1 1 d . . .
C4 C -0.3985(3) -0.1586(3) 1.0024(2) 0.0188(5) Uani 1 1 d . . .
H4 H -0.3816 -0.1762 1.0674 0.023 Uiso 1 1 calc R . .
C5 C -0.4645(3) -0.2535(2) 0.9188(2) 0.0179(5) Uani 1 1 d . . .
H5 H -0.4916 -0.3350 0.9286 0.021 Uiso 1 1 calc R . .
C6 C -0.4907(3) -0.2291(2) 0.8211(2) 0.0177(5) Uani 1 1 d . . .
C7 C -0.4485(3) -0.1066(3) 0.8068(2) 0.0210(5) Uani 1 1 d . . .
H7 H -0.4644 -0.0891 0.7417 0.025 Uiso 1 1 calc R . .
C8 C -0.3830(3) -0.0105(3) 0.8892(2) 0.0216(6) Uani 1 1 d . . .
H8 H -0.3557 0.0710 0.8793 0.026 Uiso 1 1 calc R . .
C9 C -0.5677(3) -0.3337(3) 0.7343(2) 0.0181(5) Uani 1 1 d . . .
C10 C 0.0620(3) 0.2447(3) 1.2210(2) 0.0203(5) Uani 1 1 d . . .
H10A H 0.0566 0.1643 1.2379 0.024 Uiso 1 1 calc R . .
H10B H 0.1099 0.3066 1.2817 0.024 Uiso 1 1 calc R . .
C11 C 0.1360(3) 0.2704(3) 1.1403(2) 0.0227(6) Uani 1 1 d . . .
H11A H 0.1431 0.3511 1.1233 0.027 Uiso 1 1 calc R . .
H11B H 0.2259 0.2669 1.1627 0.027 Uiso 1 1 calc R . .
C12 C 0.0671(3) 0.1914(3) 0.9602(2) 0.0184(5) Uani 1 1 d . . .
C13 C -0.0328(3) 0.1054(3) 0.8808(2) 0.0200(5) Uani 1 1 d . . .
H13 H -0.0998 0.0408 0.8940 0.024 Uiso 1 1 calc R . .
C14 C -0.0316(3) 0.1168(2) 0.7822(2) 0.0194(5) Uani 1 1 d . . .
H14 H -0.0987 0.0600 0.7291 0.023 Uiso 1 1 calc R . .
C15 C 0.0696(3) 0.2130(2) 0.7616(2) 0.0180(5) Uani 1 1 d . . .
C16 C 0.1696(3) 0.2963(2) 0.8417(2) 0.0183(5) Uani 1 1 d . . .
H16 H 0.2380 0.3596 0.8286 0.022 Uiso 1 1 calc R . .
C17 C 0.1693(3) 0.2869(3) 0.9414(2) 0.0191(5) Uani 1 1 d . . .
H17 H 0.2364 0.3435 0.9946 0.023 Uiso 1 1 calc R . .
C18 C 0.0686(3) 0.2285(3) 0.6548(2) 0.0217(6) Uani 1 1 d . . .
C19 C 0.7815(3) 0.3651(2) 0.91963(19) 0.0168(5) Uani 1 1 d . . .
C20 C 0.6663(3) 0.3965(3) 0.9057(2) 0.0208(5) Uani 1 1 d . . .
H20 H 0.6303 0.4062 0.9597 0.025 Uiso 1 1 calc R . .
C21 C 0.6046(3) 0.4133(3) 0.8104(2) 0.0192(5) Uani 1 1 d . . .
H21 H 0.5270 0.4335 0.8008 0.023 Uiso 1 1 calc R . .
C22 C 0.6588(3) 0.3998(2) 0.72962(19) 0.0149(5) Uani 1 1 d . . .
C23 C 0.7720(3) 0.3645(2) 0.7440(2) 0.0166(5) Uani 1 1 d . . .
H23 H 0.8067 0.3525 0.6897 0.020 Uiso 1 1 calc R . .
C24 C 0.8336(3) 0.3472(2) 0.8383(2) 0.0178(5) Uani 1 1 d . . .
H24 H 0.9092 0.3237 0.8472 0.021 Uiso 1 1 calc R . .
C25 C 0.5994(3) 0.4281(2) 0.62897(19) 0.0153(5) Uani 1 1 d . . .
C26 C -0.0795(3) 0.3774(3) 1.1872(2) 0.0196(5) Uani 1 1 d . . .
H26A H 0.0080 0.4340 1.1869 0.024 Uiso 1 1 calc R . .
H26B H -0.0983 0.4019 1.2498 0.024 Uiso 1 1 calc R . .
C27 C -0.1863(3) 0.3831(3) 1.0987(2) 0.0213(5) Uani 1 1 d . . .
H27A H -0.2739 0.3249 1.0969 0.026 Uiso 1 1 calc R . .
H27B H -0.1910 0.4655 1.1030 0.026 Uiso 1 1 calc R . .
C28 C 0.0233(3) 0.5551(2) 0.54444(19) 0.0155(5) Uani 1 1 d . . .
OW1 O -0.4500(3) -0.1735(2) 0.5192(2) 0.0459(7) Uani 1 1 d . . .
H1W1 H -0.4366 -0.0856 0.5429 0.055 Uiso 1 1 d . . .
H2W1 H -0.5019 -0.2137 0.5559 0.055 Uiso 1 1 d . . .
OW2 O -0.3424(4) 0.0681(3) 0.6142(3) 0.0790(13) Uani 1 1 d . . .
H1W2 H -0.3558 0.0327 0.5324 0.095 Uiso 1 1 d . . .
H2W2 H -0.4380 0.0674 0.6086 0.095 Uiso 1 1 d . . .
OW3 O -0.2526(4) 0.1588(4) 0.4623(3) 0.0758(11) Uani 1 1 d . . .
H1W3 H -0.1406 0.1770 0.4973 0.091 Uiso 1 1 d . . .
H2W3 H -0.2403 0.2617 0.4532 0.091 Uiso 1 1 d . . .
OW4 O -0.4019(6) -0.0782(4) 0.3382(4) 0.0937(14) Uani 1 1 d . . .
H1W4 H -0.4168 -0.1553 0.3744 0.112 Uiso 1 1 d . . .
H2W4 H -0.3390 0.0068 0.3987 0.112 Uiso 1 1 d . . .
OW5 O -0.0257(3) -0.0944(2) 0.59523(17) 0.0394(6) Uani 1 1 d . . .
H1W5 H -0.0024 -0.1164 0.5402 0.047 Uiso 1 1 d . . .
H2W5 H -0.0367 -0.0223 0.5926 0.047 Uiso 1 1 d . . .
OW6 O 0.2627(3) 0.2877(2) 0.45563(17) 0.0314(5) Uani 1 1 d . . .
H1W6 H 0.1847 0.2137 0.4361 0.038 Uiso 1 1 d . . .
H2W6 H 0.3267 0.2510 0.4669 0.038 Uiso 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'
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
O9 Gd1 O8 93.76(7) . 2_666 ?
O9 Gd1 O7 100.02(9) . . ?
O8 Gd1 O7 154.62(8) 2_666 . ?
O9 Gd1 OW6 74.23(8) . . ?
O8 Gd1 OW6 81.87(8) 2_666 . ?
O7 Gd1 OW6 81.54(9) . . ?
O9 Gd1 O10 147.92(7) . . ?
O8 Gd1 O10 92.56(7) 2_666 . ?
O7 Gd1 O10 87.00(9) . . ?
OW6 Gd1 O10 137.84(7) . . ?
O9 Gd1 O11 145.47(7) . 2_566 ?
O8 Gd1 O11 77.85(7) 2_666 2_566 ?
O7 Gd1 O11 78.74(8) . 2_566 ?
OW6 Gd1 O11 71.46(7) . 2_566 ?
O10 Gd1 O11 66.53(7) . 2_566 ?
O9 Gd1 O3 80.51(8) . 1_665 ?
O8 Gd1 O3 75.17(7) 2_666 1_665 ?
O7 Gd1 O3 127.94(8) . 1_665 ?
OW6 Gd1 O3 144.44(9) . 1_665 ?
O10 Gd1 O3 70.82(8) . 1_665 ?
O11 Gd1 O3 127.66(7) 2_566 1_665 ?
O9 Gd1 O2 76.88(7) . 1_665 ?
O8 Gd1 O2 127.63(7) 2_666 1_665 ?
O7 Gd1 O2 76.61(7) . 1_665 ?
OW6 Gd1 O2 139.80(7) . 1_665 ?
O10 Gd1 O2 74.40(7) . 1_665 ?
O11 Gd1 O2 134.40(6) 2_566 1_665 ?
O3 Gd1 O2 52.53(6) 1_665 1_665 ?
O9 Gd1 C9 77.17(8) . 1_665 ?
O8 Gd1 C9 101.38(8) 2_666 1_665 ?
O7 Gd1 C9 102.39(8) . 1_665 ?
OW6 Gd1 C9 151.36(8) . 1_665 ?
O10 Gd1 C9 70.76(8) . 1_665 ?
O11 Gd1 C9 137.16(7) 2_566 1_665 ?
O3 Gd1 C9 26.26(7) 1_665 1_665 ?
O2 Gd1 C9 26.28(7) 1_665 1_665 ?
C3 O1 C2 118.2(2) . . ?
C9 O2 Gd1 92.44(16) . 1_445 ?
C9 O3 Gd1 93.73(17) . 1_445 ?
C12 O4 C11 119.1(2) . . ?
C19 O5 C27 117.2(2) 1_455 . ?
C18 O7 Gd1 162.3(2) . . ?
C25 O8 Gd1 144.96(18) . 2_666 ?
C25 O9 Gd1 172.49(18) . . ?
C28 O10 Gd1 120.86(17) . . ?
C28 O11 Gd1 118.82(16) . 2_566 ?
C26 N1 C10 112.7(2) . . ?
C26 N1 C1 111.6(2) . . ?
C10 N1 C1 112.7(2) . . ?
N1 C1 C2 109.1(2) . . ?
O1 C2 C1 104.5(2) . . ?
O1 C3 C4 123.3(2) . . ?
O1 C3 C8 115.8(2) . . ?
C4 C3 C8 120.8(2) . . ?
C3 C4 C5 118.6(3) . . ?
C6 C5 C4 121.5(3) . . ?
C5 C6 C7 118.9(2) . . ?
C5 C6 C9 119.4(2) . . ?
C7 C6 C9 121.6(2) . . ?
C8 C7 C6 120.5(3) . . ?
C7 C8 C3 119.6(3) . . ?
O2 C9 O3 121.3(2) . . ?
O2 C9 C6 119.2(2) . . ?
O3 C9 C6 119.5(2) . . ?
O2 C9 Gd1 61.28(14) . 1_445 ?
O3 C9 Gd1 60.01(14) . 1_445 ?
C6 C9 Gd1 179.2(2) . 1_445 ?
N1 C10 C11 108.3(2) . . ?
O4 C11 C10 104.4(2) . . ?
O4 C12 C17 124.1(3) . . ?
O4 C12 C13 115.1(2) . . ?
C17 C12 C13 120.8(3) . . ?
C14 C13 C12 119.5(3) . . ?
C13 C14 C15 120.6(3) . . ?
C16 C15 C14 119.0(3) . . ?
C16 C15 C18 120.2(3) . . ?
C14 C15 C18 120.8(2) . . ?
C15 C16 C17 121.2(3) . . ?
C12 C17 C16 118.9(3) . . ?
O7 C18 O6 124.7(3) . . ?
O7 C18 C15 117.3(3) . . ?
O6 C18 C15 118.0(3) . . ?
O5 C19 C20 124.7(2) 1_655 . ?
O5 C19 C24 115.1(2) 1_655 . ?
C20 C19 C24 120.3(2) . . ?
C19 C20 C21 119.7(3) . . ?
C22 C21 C20 120.3(3) . . ?
C23 C22 C21 119.2(2) . . ?
C23 C22 C25 120.3(2) . . ?
C21 C22 C25 120.4(2) . . ?
C24 C23 C22 120.8(2) . . ?
C23 C24 C19 119.5(3) . . ?
O9 C25 O8 125.2(2) . . ?
O9 C25 C22 117.9(2) . . ?
O8 C25 C22 116.9(2) . . ?
N1 C26 C27 109.6(2) . . ?
O5 C27 C26 105.6(2) . . ?
O11 C28 O10 126.8(2) . . ?
O11 C28 C28 117.4(3) . 2_566 ?
O10 C28 C28 115.9(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 O9 2.296(2) . ?
Gd1 O8 2.309(2) 2_666 ?
Gd1 O7 2.316(2) . ?
Gd1 OW6 2.405(2) . ?
Gd1 O10 2.413(2) . ?
Gd1 O11 2.461(2) 2_566 ?
Gd1 O3 2.477(2) 1_665 ?
Gd1 O2 2.505(2) 1_665 ?
Gd1 C9 2.853(3) 1_665 ?
O1 C3 1.372(3) . ?
O1 C2 1.437(3) . ?
O2 C9 1.264(3) . ?
O2 Gd1 2.505(2) 1_445 ?
O3 C9 1.265(3) . ?
O3 Gd1 2.477(2) 1_445 ?
O4 C12 1.375(3) . ?
O4 C11 1.437(4) . ?
O5 C19 1.376(3) 1_455 ?
O5 C27 1.431(3) . ?
O6 C18 1.264(4) . ?
O7 C18 1.250(4) . ?
O8 C25 1.251(3) . ?
O8 Gd1 2.309(2) 2_666 ?
O9 C25 1.248(3) . ?
O10 C28 1.258(3) . ?
O11 C28 1.244(3) . ?
O11 Gd1 2.461(2) 2_566 ?
N1 C26 1.502(3) . ?
N1 C10 1.503(4) . ?
N1 C1 1.507(3) . ?
C1 C2 1.516(4) . ?
C3 C4 1.392(4) . ?
C3 C8 1.393(4) . ?
C4 C5 1.394(4) . ?
C5 C6 1.389(4) . ?
C6 C7 1.396(4) . ?
C6 C9 1.496(4) . ?
C7 C8 1.391(4) . ?
C9 Gd1 2.853(3) 1_445 ?
C10 C11 1.515(4) . ?
C12 C17 1.390(4) . ?
C12 C13 1.394(4) . ?
C13 C14 1.382(4) . ?
C14 C15 1.400(4) . ?
C15 C16 1.388(4) . ?
C15 C18 1.501(4) . ?
C16 C17 1.392(4) . ?
C19 O5 1.376(3) 1_655 ?
C19 C20 1.388(4) . ?
C19 C24 1.394(4) . ?
C20 C21 1.396(4) . ?
C21 C22 1.392(4) . ?
C22 C23 1.393(4) . ?
C22 C25 1.506(3) . ?
C23 C24 1.386(4) . ?
C26 C27 1.505(4) . ?
C28 C28 1.552(5) 2_566 ?
