More examples of the 15-crown-5···H~2~O—<i>M</i>—OH~2~···15-crown-5 motif, <i>M</i> = Al^3+^, Cr^3+^ and Pd^2+^
Siegler, Maxime A.; Prewitt, Jacob H.; Kelley, Steven P.; Parkin, Sean; Selegue, John P.; Brock, Carolyn Pratt; Acta Crystallographica Section B 66 (2010) 213–221; doi:10.1107/S0108768110007202

data_2104708
_publ_section_title
;
 More examples of the
 15-crown-5&#x00B7;&#x00B7;&#x00B7;H~2~O---<i>M</i>---OH~2~&#x00B7;&#x00B7;&#x00B7;15-crown-5
 motif, <i>M</i> = Al^3+^, Cr^3+^ and Pd^2+^
;
_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, Al H12 O6, 3(N O3), 4(H2 O)'
_chemical_formula_sum            'C10 H40 Al N3 O24'
_chemical_formula_weight         613.43
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 99.3468(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.6039(3)
_cell_length_b                   9.36110(10)
_cell_length_c                   31.5795(5)
_cell_measurement_reflns_used    6560
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     5426.65(14)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            40687
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.475
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6212
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0422
_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/[\s^2^(Fo^2^)+(0.0561P)^2^+1.7455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                4125
_reflns_number_total             6212
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            zb5012.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2104708
_cod_database_fobs_code          2104708