#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/95/7019575.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_7019575
loop_
_publ_author_name
'Merkens, Carina'
'Becker, Nils'
'Lamberts, Kevin'
'Englert, Ulli'
_publ_section_title
;
 Bimetallic coordination networks based on Al(acacCN)(3): a building block
 between inertness and lability.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8594
_journal_page_last               8599
_journal_paper_doi               10.1039/c2dt30623a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C13 H15 Ag0.5 Al N2 O5, 5(H2 O), 0.5(O H)'
_chemical_formula_sum            'C13 H26.5 Ag0.5 Al N2 O11'
_chemical_formula_weight         467.78
_chemical_name_common            3c_100K
_chemical_name_systematic
;
?
;
_space_group_IT_number           49
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2c'
_symmetry_space_group_name_H-M   'P c c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5718(10)
_cell_length_b                   10.8468(15)
_cell_length_c                   23.771(3)
_cell_measurement_reflns_used    2170
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.70
_cell_measurement_theta_min      2.54
_cell_volume                     1952.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21738
_diffrn_reflns_theta_full        26.67
_diffrn_reflns_theta_max         26.67
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.9379
_exptl_absorpt_correction_T_min  0.8920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
refinement of the expected constituents resulted in
unsatisfactory agreement, in particular with respect to
low resoltion reflection. Difference Fourier syntheses
did not allow to construct a chemically meaningful
disorder model. Most likely, the voids contain one
hydroxide counteranion and 11 water molecules per formula
unit; this assignment is in reasonable agreement with
electron count, void volume and results from thermal
analyses.
;
_refine_diff_density_max         0.913
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0615
_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)+(0.0515P)²+7.0946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1547
_reflns_number_gt                1636
_reflns_number_total             2114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30623a.txt
_cod_data_source_block           3c_100K
_cod_original_cell_volume        1952.3(5)
_cod_original_formula_sum        'C13 H26.50 Ag0.50 Al N2 O11'
_cod_database_code               7019575
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
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
Ag1 Ag 0.0000 0.5000 0.2500 0.0426(3) Uani 1 4 d S
Al1 Al 0.5000 0.0000 0.43998(8) 0.0352(4) Uani 1 2 d S
O1 O 0.2693(4) 0.0675(3) 0.43422(14) 0.0360(7) Uani 1 1 d .
O2 O 0.5761(4) 0.1157(4) 0.38583(15) 0.0502(10) Uani 1 1 d .
O3 O 0.5624(5) 0.0979(4) 0.5000 0.0322(10) Uani 1 2 d S
C1 C 0.0181(7) 0.1820(6) 0.4124(3) 0.0573(15) Uani 1 1 d .
H1A H -0.0434 0.1613 0.3774 0.086 Uiso 1 1 calc R
H1B H 0.0019 0.2699 0.4206 0.086 Uiso 1 1 calc R
H1C H -0.0305 0.1328 0.4433 0.086 Uiso 1 1 calc R
C2 C 0.2093(6) 0.1550(4) 0.4062(2) 0.0355(10) Uani 1 1 d .
C3 C 0.3162(6) 0.2249(5) 0.3691(2) 0.0397(11) Uani 1 1 d .
C4 C 0.4952(7) 0.2054(5) 0.3622(2) 0.0470(12) Uani 1 1 d .
C5 C 0.6085(8) 0.2886(7) 0.3265(3) 0.076(2) Uani 1 1 d .
H5A H 0.6678 0.3492 0.3505 0.114 Uiso 1 1 calc R
H5B H 0.5341 0.3315 0.2990 0.114 Uiso 1 1 calc R
H5C H 0.6972 0.2392 0.3067 0.114 Uiso 1 1 calc R
C6 C 0.2373(7) 0.3200(6) 0.3370(3) 0.0561(15) Uani 1 1 d .
C7 C 0.617(3) 0.239(2) 0.5000 0.204(12) Uani 1 2 d S
H7A H 0.6944 0.2567 0.5320 0.306 Uiso 1 1 d R
H7B H 0.5094 0.2894 0.5000 0.306 Uiso 1 2 d SR
N1 N 0.1695(7) 0.3934(5) 0.3098(3) 0.0804(19) 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'
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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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'
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
N1 Ag1 N1 109.9(3) 3 2_565
N1 Ag1 N1 101.1(3) 3 4_565
N1 Ag1 N1 117.8(4) 2_565 4_565
N1 Ag1 N1 117.8(4) 3 .
N1 Ag1 N1 101.1(3) 2_565 .
N1 Ag1 N1 109.9(3) 4_565 .
O3 Al1 O3 78.3(2) 5_656 .
O3 Al1 O2 172.14(18) 5_656 .
O3 Al1 O2 93.83(16) . .
O3 Al1 O2 93.83(16) 5_656 2_655
O3 Al1 O2 172.14(18) . 2_655
O2 Al1 O2 94.0(3) . 2_655
O3 Al1 O1 92.42(17) 5_656 .
O3 Al1 O1 93.99(17) . .
O2 Al1 O1 88.60(14) . .
O2 Al1 O1 85.76(15) 2_655 .
O3 Al1 O1 93.99(17) 5_656 2_655
O3 Al1 O1 92.42(17) . 2_655
O2 Al1 O1 85.77(15) . 2_655
O2 Al1 O1 88.60(14) 2_655 2_655
O1 Al1 O1 171.7(2) . 2_655
O3 Al1 Al1 39.16(11) 5_656 5_656
O3 Al1 Al1 39.16(11) . 5_656
O2 Al1 Al1 132.99(13) . 5_656
O2 Al1 Al1 132.99(13) 2_655 5_656
O1 Al1 Al1 94.13(11) . 5_656
O1 Al1 Al1 94.13(11) 2_655 5_656
C2 O1 Al1 131.9(3) . .
C4 O2 Al1 131.2(3) . .
C7 O3 Al1 128.60(14) . .
C7 O3 Al1 128.60(14) . 5_656
Al1 O3 Al1 101.7(2) . 5_656
C2 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O1 C2 C3 122.2(4) . .
O1 C2 C1 116.9(5) . .
C3 C2 C1 120.9(4) . .
C4 C3 C6 117.5(5) . .
C4 C3 C2 123.5(5) . .
C6 C3 C2 119.0(4) . .
O2 C4 C3 122.3(5) . .
O2 C4 C5 115.5(5) . .
C3 C4 C5 122.2(5) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N1 C6 C3 177.2(7) . .
O3 C7 H7A 109.9 . .
O3 C7 H7B 108.7 . .
H7A C7 H7B 113.1 . .
C6 N1 Ag1 166.8(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N1 2.236(5) 3
Ag1 N1 2.236(5) 2_565
Ag1 N1 2.236(5) 4_565
Ag1 N1 2.236(5) .
Al1 O3 1.840(3) 5_656
Al1 O3 1.840(3) .
Al1 O2 1.888(4) .
Al1 O2 1.888(4) 2_655
Al1 O1 1.899(3) .
Al1 O1 1.899(3) 2_655
Al1 Al1 2.854(4) 5_656
O1 C2 1.246(5) .
O2 C4 1.279(6) .
O3 C7 1.59(2) .
O3 Al1 1.840(3) 5_656
C1 C2 1.485(6) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 C3 1.416(7) .
C3 C4 1.382(7) .
C3 C6 1.416(7) .
C4 C5 1.508(8) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 N1 1.147(7) .
C7 H7A 0.9800 .
C7 H7B 0.9772 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.024 0.000 0.250 122 63 '5 H2O, OH- '
2 -0.024 0.000 0.750 122 63 '5 H2O, OH- '
3 -0.041 0.500 0.000 155 61 '6 H2O'
4 -0.024 0.500 0.500 155 61 '6 H2O'
