#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/47/2104710.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2104710
loop_
_publ_author_name
'Siegler, Maxime A.'
'Prewitt, Jacob H.'
'Kelley, Steven P.'
'Parkin, Sean'
'Selegue, John P.'
'Brock, Carolyn Pratt'
_publ_section_title
;
 More examples of the
 15-crown-5···H₂O---M---OH₂···15-crown-5
 motif, M = Al³⁺, Cr³⁺ and Pd²⁺
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              213
_journal_page_last               221
_journal_paper_doi               10.1107/S0108768110007202
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C10 H20 O5, H4 N2 O8 Pd'
_chemical_formula_sum            'C10 H24 N2 O13 Pd'
_chemical_formula_weight         486.71
_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                73.8388(7)
_cell_angle_beta                 88.0601(7)
_cell_angle_gamma                73.6959(7)
_cell_formula_units_Z            2
_cell_length_a                   7.46490(10)
_cell_length_b                   9.54870(10)
_cell_length_c                   13.3944(2)
_cell_measurement_reflns_used    3994
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     879.13(2)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELX-97 (Sheldrick, 2008) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'ω scans at fixed χ = 55°'
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21461
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.802
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4016
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0150P)²+0.7189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0516
_reflns_number_gt                3440
_reflns_number_total             4016
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            zb5012.cif
_cod_data_source_block           4
_cod_database_code               2104710
_cod_database_fobs_code          2104710
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.44978(18) 0.84124(14) 0.21893(10) 0.0138(3) Uani d . 1 . .
O O2 0.10662(17) 0.94188(14) 0.29899(9) 0.0132(3) Uani d . 1 . .
O O3 -0.00280(17) 0.68012(14) 0.37128(10) 0.0137(3) Uani d . 1 . .
O O4 0.03914(19) 0.55976(15) 0.19211(10) 0.0174(3) Uani d . 1 . .
O O5 0.36269(17) 0.63634(14) 0.11768(10) 0.0153(3) Uani d . 1 . .
C C1 0.3756(3) 0.9976(2) 0.21703(15) 0.0154(4) Uani d . 1 . .
H H1A 0.2999 1.0555 0.1517 0.018 Uiso calc R 1 . .
H H1B 0.4786 1.0427 0.2208 0.018 Uiso calc R 1 . .
C C2 0.2561(3) 1.0043(2) 0.30908(15) 0.0145(4) Uani d . 1 . .
H H2A 0.3315 0.9452 0.3744 0.017 Uiso calc R 1 . .
H H2B 0.2053 1.1110 0.3112 0.017 Uiso calc R 1 . .
C C3 -0.0034(3) 0.9215(2) 0.38901(14) 0.0156(4) Uani d . 1 . .
H H3A -0.0829 1.0212 0.3941 0.019 Uiso calc R 1 . .
H H3B 0.0792 0.8723 0.4528 0.019 Uiso calc R 1 . .
C C4 -0.1233(3) 0.8230(2) 0.37831(15) 0.0166(4) Uani d . 1 . .
H H4A -0.2013 0.8069 0.4394 0.020 Uiso calc R 1 . .
H H4B -0.2070 0.8728 0.3150 0.020 Uiso calc R 1 . .
C C5 -0.0982(3) 0.5780(2) 0.35249(15) 0.0175(4) Uani d . 1 . .
H H5A -0.2144 0.6370 0.3095 0.021 Uiso calc R 1 . .
H H5B -0.1328 0.5182 0.4195 0.021 Uiso calc R 1 . .
C C6 0.0246(3) 0.4727(2) 0.29743(15) 0.0179(4) Uani d . 1 . .
H H6A 0.1500 0.4275 0.3332 0.021 Uiso calc R 1 . .
H H6B -0.0299 0.3895 0.2974 0.021 Uiso calc R 1 . .
C C7 0.1660(3) 0.4764(2) 0.13249(16) 0.0179(4) Uani d . 1 . .
H H7A 0.1250 0.5193 0.0580 0.021 Uiso calc R 1 . .
H H7B 0.1623 0.3693 0.1541 0.021 Uiso calc R 1 . .
C C8 0.3648(3) 0.4807(2) 0.14576(15) 0.0157(4) Uani d . 1 . .
H H8A 0.4119 0.4304 0.2189 0.019 Uiso calc R 1 . .
H H8B 0.4472 0.4271 0.1004 0.019 Uiso calc R 1 . .
C C9 0.5438(3) 0.6568(2) 0.12320(15) 0.0167(4) Uani d . 1 . .
H H9A 0.6153 0.6342 0.0632 0.020 Uiso calc R 1 . .
H H9B 0.6132 0.5870 0.1880 0.020 Uiso calc R 1 . .
C C10 0.5201(3) 0.8192(2) 0.12174(14) 0.0143(4) Uani d . 1 . .
H H10A 0.6418 0.8423 0.1110 0.017 Uiso calc R 1 . .
H H10B 0.4318 0.8887 0.0638 0.017 Uiso calc R 1 . .
Pd Pd1 0.5000 0.5000 0.5000 0.00905(6) Uani d S 1 . .
O O61 0.36808(19) 0.61191(15) 0.35964(10) 0.0152(3) Uani d D 1 . .
H H61A 0.397(3) 0.680(2) 0.3221(17) 0.023 Uiso d D 1 . .
H H61B 0.262(3) 0.633(3) 0.3622(18) 0.023 Uiso d D 1 . .
O O71 0.44716(18) 0.31460(15) 0.48166(10) 0.0164(3) Uani d . 1 . .
N N1 0.5632(2) 0.24692(17) 0.42048(12) 0.0145(3) Uani d . 1 . .
O O81 0.7008(2) 0.29036(16) 0.39221(11) 0.0211(3) Uani d . 1 . .
O O91 0.5235(2) 0.14365(17) 0.39839(12) 0.0275(3) Uani d . 1 . .
Pd Pd2 0.0000 1.0000 0.0000 0.00852(6) Uani d S 1 . .
O O62 -0.0070(2) 0.86094(15) 0.14265(10) 0.0157(3) Uani d D 1 . .
H H62A 0.042(3) 0.882(3) 0.1853(17) 0.024 Uiso d D 1 . .
H H62B 0.040(3) 0.776(2) 0.1489(18) 0.024 Uiso d D 1 . .
O O72 -0.01441(17) 1.17356(14) 0.05803(10) 0.0133(3) Uani d . 1 . .
N N2 -0.1691(2) 1.21875(17) 0.10712(12) 0.0133(3) Uani d . 1 . .
O O82 -0.29127(19) 1.15441(15) 0.11248(11) 0.0189(3) Uani d . 1 . .
O O92 -0.1755(2) 1.32423(16) 0.14308(12) 0.0241(3) Uani d . 1 . .
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'
Pd Pd -0.9988 1.0072 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 O1 C10 . . 113.95(14) ?
C2 O2 C3 . . 113.95(14) ?
C4 O3 C5 . . 114.57(14) ?
C7 O4 C6 . . 114.13(14) ?
C8 O5 C9 . . 113.12(14) ?
O1 C1 C2 . . 107.99(14) ?
O1 C1 H1A . . 110.1 ?
C2 C1 H1A . . 110.1 ?
O1 C1 H1B . . 110.1 ?
C2 C1 H1B . . 110.1 ?
H1A C1 H1B . . 108.4 ?
O2 C2 C1 . . 108.15(15) ?
O2 C2 H2A . . 110.1 ?
C1 C2 H2A . . 110.1 ?
O2 C2 H2B . . 110.1 ?
C1 C2 H2B . . 110.1 ?
H2A C2 H2B . . 108.4 ?
O2 C3 C4 . . 108.11(15) ?
O2 C3 H3A . . 110.1 ?
C4 C3 H3A . . 110.1 ?
O2 C3 H3B . . 110.1 ?
C4 C3 H3B . . 110.1 ?
H3A C3 H3B . . 108.4 ?
O3 C4 C3 . . 108.23(15) ?
O3 C4 H4A . . 110.1 ?
C3 C4 H4A . . 110.1 ?
O3 C4 H4B . . 110.1 ?
C3 C4 H4B . . 110.1 ?
H4A C4 H4B . . 108.4 ?
O3 C5 C6 . . 110.22(15) ?
O3 C5 H5A . . 109.6 ?
C6 C5 H5A . . 109.6 ?
O3 C5 H5B . . 109.6 ?
C6 C5 H5B . . 109.6 ?
H5A C5 H5B . . 108.1 ?
O4 C6 C5 . . 107.93(15) ?
O4 C6 H6A . . 110.1 ?
C5 C6 H6A . . 110.1 ?
O4 C6 H6B . . 110.1 ?
C5 C6 H6B . . 110.1 ?
H6A C6 H6B . . 108.4 ?
O4 C7 C8 . . 112.45(16) ?
O4 C7 H7A . . 109.1 ?
C8 C7 H7A . . 109.1 ?
O4 C7 H7B . . 109.1 ?
C8 C7 H7B . . 109.1 ?
H7A C7 H7B . . 107.8 ?
O5 C8 C7 . . 107.28(15) ?
O5 C8 H8A . . 110.3 ?
C7 C8 H8A . . 110.3 ?
O5 C8 H8B . . 110.3 ?
C7 C8 H8B . . 110.3 ?
H8A C8 H8B . . 108.5 ?
O5 C9 C10 . . 108.22(15) ?
O5 C9 H9A . . 110.1 ?
C10 C9 H9A . . 110.1 ?
O5 C9 H9B . . 110.1 ?
C10 C9 H9B . . 110.1 ?
H9A C9 H9B . . 108.4 ?
O1 C10 C9 . . 109.12(14) ?
O1 C10 H10A . . 109.9 ?
C9 C10 H10A . . 109.9 ?
O1 C10 H10B . . 109.9 ?
C9 C10 H10B . . 109.9 ?
H10A C10 H10B . . 108.3 ?
O71 Pd1 O71 . 2_666 180.0 ?
O71 Pd1 O61 . 2_666 93.08(5) ?
O71 Pd1 O61 2_666 2_666 86.92(5) ?
O71 Pd1 O61 . . 86.92(5) ?
O71 Pd1 O61 2_666 . 93.08(5) ?
O61 Pd1 O61 2_666 . 179.9990(10) ?
Pd1 O61 H61A . . 121.4(17) ?
Pd1 O61 H61B . . 112.6(18) ?
H61A O61 H61B . . 110(2) ?
N1 O71 Pd1 . . 114.36(10) ?
O91 N1 O81 . . 125.14(16) ?
O91 N1 O71 . . 116.21(15) ?
O81 N1 O71 . . 118.63(15) ?
O72 Pd2 O72 . 2_575 180.00(7) ?
O72 Pd2 O62 . . 91.55(5) ?
O72 Pd2 O62 2_575 . 88.45(5) ?
O72 Pd2 O62 . 2_575 88.45(5) ?
O72 Pd2 O62 2_575 2_575 91.55(5) ?
O62 Pd2 O62 . 2_575 179.9990(10) ?
Pd2 O62 H62A . . 111.9(18) ?
Pd2 O62 H62B . . 115.3(18) ?
H62A O62 H62B . . 106(2) ?
N2 O72 Pd2 . . 115.97(10) ?
O92 N2 O82 . . 125.46(16) ?
O92 N2 O72 . . 115.34(15) ?
O82 N2 O72 . . 119.20(15) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 . 1.432(2) ?
O1 C10 . 1.435(2) ?
O2 C2 . 1.431(2) ?
O2 C3 . 1.435(2) ?
O3 C4 . 1.434(2) ?
O3 C5 . 1.435(2) ?
O4 C7 . 1.431(2) ?
O4 C6 . 1.442(2) ?
O5 C8 . 1.424(2) ?
O5 C9 . 1.426(2) ?
C1 C2 . 1.502(3) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.504(3) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C6 . 1.498(3) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.513(3) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C10 . 1.506(3) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
Pd1 O71 . 1.9977(13) ?
Pd1 O71 2_666 1.9977(13) ?
Pd1 O61 2_666 2.0155(13) ?
Pd1 O61 . 2.0155(13) ?
O61 H61A . 0.784(18) ?
O61 H61B . 0.765(18) ?
O71 N1 . 1.331(2) ?
N1 O91 . 1.216(2) ?
N1 O81 . 1.224(2) ?
Pd2 O72 . 1.9934(12) ?
Pd2 O72 2_575 1.9935(12) ?
Pd2 O62 . 2.0091(13) ?
Pd2 O62 2_575 2.0091(13) ?
O62 H62A . 0.784(18) ?
O62 H62B . 0.770(18) ?
O72 N2 . 1.3335(19) ?
N2 O92 . 1.221(2) ?
N2 O82 . 1.225(2) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C10 O1 C1 C2 . . . . 162.68(14) ?
C3 O2 C2 C1 . . . . 171.64(14) ?
O1 C1 C2 O2 . . . . -61.31(18) ?
C2 O2 C3 C4 . . . . -166.83(15) ?
C5 O3 C4 C3 . . . . -175.34(15) ?
O2 C3 C4 O3 . . . . 59.79(19) ?
C4 O3 C5 C6 . . . . 152.96(15) ?
C7 O4 C6 C5 . . . . 174.84(15) ?
O3 C5 C6 O4 . . . . -71.36(19) ?
C6 O4 C7 C8 . . . . -87.05(19) ?
C9 O5 C8 C7 . . . . -177.92(15) ?
O4 C7 C8 O5 . . . . -56.6(2) ?
C8 O5 C9 C10 . . . . -164.40(15) ?
C1 O1 C10 C9 . . . . -164.36(15) ?
O5 C9 C10 O1 . . . . 71.00(18) ?
O61 Pd1 O71 N1 2_666 . . . -100.46(12) ?
O61 Pd1 O71 N1 . . . . 79.54(12) ?
Pd1 O71 N1 O91 . . . . -172.34(12) ?
Pd1 O71 N1 O81 . . . . 8.7(2) ?
O62 Pd2 O72 N2 . . . . -62.55(12) ?
O62 Pd2 O72 N2 2_575 . . . 117.45(12) ?
Pd2 O72 N2 O92 . . . . 179.39(12) ?
Pd2 O72 N2 O82 . . . . -1.0(2) ?
