#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/47/2104711.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_2104711
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
'2(C10 H20 O5), H4 N2 O8 Pd, 2(H N O3), 2(H2 O)'
_chemical_formula_sum            'C20 H50 N4 O26 Pd'
_chemical_formula_weight         869.04
_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                79.8454(9)
_cell_angle_beta                 87.7567(9)
_cell_angle_gamma                70.4587(11)
_cell_formula_units_Z            1
_cell_length_a                   7.00480(10)
_cell_length_b                   9.8871(2)
_cell_length_c                   13.8440(3)
_cell_measurement_reflns_used    7640
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     889.21(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0397
_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            24163
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.781
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0244
_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)+(0.0166P)²+0.5279P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0626
_reflns_number_gt                3946
_reflns_number_total             4040
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            zb5012.cif
_cod_data_source_block           5
_cod_database_code               2104711
_cod_database_fobs_code          2104711
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 0.44859(18) 0.76046(12) 0.26456(8) 0.0179(2) Uani d . 1 . .
O O2 0.50643(16) 0.47734(11) 0.37780(8) 0.0157(2) Uani d . 1 . .
O O3 0.32545(16) 0.36081(11) 0.25227(8) 0.0146(2) Uani d . 1 . .
O O4 0.00778(16) 0.60402(11) 0.17921(8) 0.0151(2) Uani d . 1 . .
O O5 0.18429(17) 0.82662(11) 0.10688(8) 0.0170(2) Uani d . 1 . .
C C1 0.5224(2) 0.71708(17) 0.36298(11) 0.0175(3) Uani d . 1 . .
H H1A 0.4081 0.7348 0.4088 0.021 Uiso calc R 1 . .
H H1B 0.6091 0.7734 0.3759 0.021 Uiso calc R 1 . .
C C2 0.6438(2) 0.55676(17) 0.37717(12) 0.0174(3) Uani d . 1 . .
H H2A 0.7405 0.5366 0.3232 0.021 Uiso calc R 1 . .
H H2B 0.7216 0.5267 0.4400 0.021 Uiso calc R 1 . .
C C3 0.5995(2) 0.33242(16) 0.35770(11) 0.0159(3) Uani d . 1 . .
H H3A 0.6866 0.2696 0.4141 0.019 Uiso calc R 1 . .
H H3B 0.6847 0.3339 0.2990 0.019 Uiso calc R 1 . .
C C4 0.4330(2) 0.27459(16) 0.34020(11) 0.0164(3) Uani d . 1 . .
H H4A 0.4908 0.1710 0.3327 0.020 Uiso calc R 1 . .
H H4B 0.3402 0.2817 0.3963 0.020 Uiso calc R 1 . .
C C5 0.1311(2) 0.34818(16) 0.23942(12) 0.0167(3) Uani d . 1 . .
H H5A 0.0533 0.3596 0.3005 0.020 Uiso calc R 1 . .
H H5B 0.1469 0.2510 0.2240 0.020 Uiso calc R 1 . .
C C6 0.0208(2) 0.46584(16) 0.15624(12) 0.0162(3) Uani d . 1 . .
H H6A 0.0948 0.4510 0.0945 0.019 Uiso calc R 1 . .
H H6B -0.1168 0.4622 0.1473 0.019 Uiso calc R 1 . .
C C7 -0.0763(2) 0.72315(17) 0.10046(12) 0.0189(3) Uani d . 1 . .
H H7A -0.2248 0.7462 0.0958 0.023 Uiso calc R 1 . .
H H7B -0.0172 0.6968 0.0375 0.023 Uiso calc R 1 . .
C C8 -0.0287(2) 0.85312(17) 0.12069(12) 0.0183(3) Uani d . 1 . .
H H8A -0.1083 0.9418 0.0753 0.022 Uiso calc R 1 . .
H H8B -0.0644 0.8681 0.1888 0.022 Uiso calc R 1 . .
C C9 0.2528(3) 0.93496(16) 0.13642(12) 0.0194(3) Uani d . 1 . .
H H9A 0.1461 1.0315 0.1202 0.023 Uiso calc R 1 . .
H H9B 0.3748 0.9392 0.0992 0.023 Uiso calc R 1 . .
C C10 0.3027(3) 0.90252(16) 0.24537(11) 0.0179(3) Uani d . 1 . .
H H10A 0.3585 0.9747 0.2632 0.022 Uiso calc R 1 . .
H H10B 0.1795 0.9061 0.2839 0.022 Uiso calc R 1 . .
Pd Pd 0.5000 0.5000 0.0000 0.01145(6) Uani d S 1 . .
O O61 0.46157(17) 0.55162(12) 0.13540(8) 0.0148(2) Uani d D 1 . .
H H61A 0.412(3) 0.497(2) 0.1710(14) 0.022 Uiso d D 1 . .
H H61B 0.385(3) 0.6339(18) 0.1310(15) 0.022 Uiso d D 1 . .
N N1 0.4049(2) 0.78769(14) -0.10510(10) 0.0167(3) Uani d . 1 . .
O O71 0.54243(17) 0.69096(12) -0.04279(8) 0.0174(2) Uani d . 1 . .
O O81 0.25517(18) 0.76050(12) -0.12672(9) 0.0211(2) Uani d . 1 . .
O O91 0.4395(2) 0.90026(13) -0.13799(10) 0.0275(3) Uani d . 1 . .
O O11 0.09790(18) 0.61520(13) 0.36789(8) 0.0172(2) Uani d D 1 . .
H H11B 0.055(3) 0.624(2) 0.3153(13) 0.026 Uiso d D 1 . .
H H11A 0.218(3) 0.582(2) 0.3672(15) 0.026 Uiso d D 1 . .
N N2 -0.1473(2) 0.90971(14) 0.46176(10) 0.0177(3) Uani d . 1 . .
O O14 -0.1678(2) 0.94905(13) 0.37352(9) 0.0252(3) Uani d . 1 . .
O O15 -0.2131(2) 0.98334(14) 0.52467(10) 0.0292(3) Uani d . 1 . .
O O16 -0.04218(19) 0.76821(12) 0.49542(8) 0.0201(2) Uani d . 1 . .
H H16 -0.004(3) 0.729(2) 0.4462(17) 0.030 Uiso 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 . . 113.60(11) ?
C2 O2 C3 . . 113.94(12) ?
C5 O3 C4 . . 114.50(12) ?
C6 O4 C7 . . 113.31(11) ?
C9 O5 C8 . . 113.28(12) ?
O1 C1 C2 . . 107.55(12) ?
O1 C1 H1A . . 110.2 ?
C2 C1 H1A . . 110.2 ?
O1 C1 H1B . . 110.2 ?
C2 C1 H1B . . 110.2 ?
H1A C1 H1B . . 108.5 ?
O2 C2 C1 . . 108.35(12) ?
O2 C2 H2A . . 110.0 ?
C1 C2 H2A . . 110.0 ?
O2 C2 H2B . . 110.0 ?
C1 C2 H2B . . 110.0 ?
H2A C2 H2B . . 108.4 ?
O2 C3 C4 . . 107.70(12) ?
O2 C3 H3A . . 110.2 ?
C4 C3 H3A . . 110.2 ?
O2 C3 H3B . . 110.2 ?
C4 C3 H3B . . 110.2 ?
H3A C3 H3B . . 108.5 ?
O3 C4 C3 . . 107.45(12) ?
O3 C4 H4A . . 110.2 ?
C3 C4 H4A . . 110.2 ?
O3 C4 H4B . . 110.2 ?
C3 C4 H4B . . 110.2 ?
H4A C4 H4B . . 108.5 ?
O3 C5 C6 . . 108.12(12) ?
O3 C5 H5A . . 110.1 ?
C6 C5 H5A . . 110.1 ?
O3 C5 H5B . . 110.1 ?
C6 C5 H5B . . 110.1 ?
H5A C5 H5B . . 108.4 ?
O4 C6 C5 . . 108.60(12) ?
O4 C6 H6A . . 110.0 ?
C5 C6 H6A . . 110.0 ?
O4 C6 H6B . . 110.0 ?
C5 C6 H6B . . 110.0 ?
H6A C6 H6B . . 108.4 ?
O4 C7 C8 . . 108.40(12) ?
O4 C7 H7A . . 110.0 ?
C8 C7 H7A . . 110.0 ?
O4 C7 H7B . . 110.0 ?
C8 C7 H7B . . 110.0 ?
H7A C7 H7B . . 108.4 ?
O5 C8 C7 . . 108.25(12) ?
O5 C8 H8A . . 110.0 ?
C7 C8 H8A . . 110.0 ?
O5 C8 H8B . . 110.0 ?
C7 C8 H8B . . 110.0 ?
H8A C8 H8B . . 108.4 ?
O5 C9 C10 . . 111.89(12) ?
O5 C9 H9A . . 109.2 ?
C10 C9 H9A . . 109.2 ?
O5 C9 H9B . . 109.2 ?
C10 C9 H9B . . 109.2 ?
H9A C9 H9B . . 107.9 ?
O1 C10 C9 . . 106.47(12) ?
O1 C10 H10A . . 110.4 ?
C9 C10 H10A . . 110.4 ?
O1 C10 H10B . . 110.4 ?
C9 C10 H10B . . 110.4 ?
H10A C10 H10B . . 108.6 ?
O71 Pd O71 2_665 . 180.0 ?
O71 Pd O61 2_665 . 93.61(4) ?
O71 Pd O61 . . 86.39(4) ?
O71 Pd O61 2_665 2_665 86.39(4) ?
O71 Pd O61 . 2_665 93.61(4) ?
O61 Pd O61 . 2_665 180.0000(10) ?
Pd O61 H61A . . 109.9(14) ?
Pd O61 H61B . . 108.2(14) ?
H61A O61 H61B . . 109.2(19) ?
O91 N1 O81 . . 124.53(14) ?
O91 N1 O71 . . 115.88(13) ?
O81 N1 O71 . . 119.59(12) ?
N1 O71 Pd . . 115.71(9) ?
H11B O11 H11A . . 109(2) ?
O15 N2 O14 . . 127.20(14) ?
O15 N2 O16 . . 115.15(14) ?
O14 N2 O16 . . 117.65(12) ?
N2 O16 H16 . . 106.8(16) ?
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 . 1.4173(18) ?
O1 C10 . 1.4203(18) ?
O2 C2 . 1.4298(18) ?
O2 C3 . 1.4342(17) ?
O3 C5 . 1.4284(17) ?
O3 C4 . 1.4325(17) ?
O4 C6 . 1.4296(17) ?
O4 C7 . 1.4339(18) ?
O5 C9 . 1.4346(17) ?
O5 C8 . 1.4373(19) ?
C1 C2 . 1.508(2) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 C4 . 1.505(2) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C5 C6 . 1.508(2) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C6 H6A . 0.9900 ?
C6 H6B . 0.9900 ?
C7 C8 . 1.504(2) ?
C7 H7A . 0.9900 ?
C7 H7B . 0.9900 ?
C8 H8A . 0.9900 ?
C8 H8B . 0.9900 ?
C9 C10 . 1.515(2) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
Pd O71 2_665 1.9928(11) ?
Pd O71 . 1.9928(11) ?
Pd O61 . 2.0131(10) ?
Pd O61 2_665 2.0132(10) ?
O61 H61A . 0.824(16) ?
O61 H61B . 0.803(16) ?
N1 O91 . 1.2238(17) ?
N1 O81 . 1.2260(17) ?
N1 O71 . 1.3210(17) ?
O11 H11B . 0.778(17) ?
O11 H11A . 0.795(17) ?
N2 O15 . 1.2118(18) ?
N2 O14 . 1.2137(18) ?
N2 O16 . 1.3506(17) ?
O16 H16 . 0.84(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 . . . . 169.59(13) ?
C3 O2 C2 C1 . . . . 160.14(12) ?
O1 C1 C2 O2 . . . . -71.58(15) ?
C2 O2 C3 C4 . . . . -168.49(12) ?
C5 O3 C4 C3 . . . . -163.46(12) ?
O2 C3 C4 O3 . . . . 65.60(15) ?
C4 O3 C5 C6 . . . . 168.73(12) ?
C7 O4 C6 C5 . . . . 173.98(12) ?
O3 C5 C6 O4 . . . . -57.44(15) ?
C6 O4 C7 C8 . . . . -164.09(13) ?
C9 O5 C8 C7 . . . . -172.38(12) ?
O4 C7 C8 O5 . . . . 71.41(16) ?
C8 O5 C9 C10 . . . . 84.82(16) ?
C1 O1 C10 C9 . . . . 175.87(12) ?
O5 C9 C10 O1 . . . . 56.16(17) ?
O91 N1 O71 Pd . . . . -174.00(10) ?
O81 N1 O71 Pd . . . . 5.52(16) ?
O61 Pd O71 N1 . . . . -115.14(10) ?
O61 Pd O71 N1 2_665 . . . 64.86(10) ?
