#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:28:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179482 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/79/4337994.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_4337994
loop_
_publ_author_name
'Chyba, Jan'
'Moravec, Zdenek'
'Necas, Marek'
'Mathur, Sanjay'
'Pinkas, Jiri'
_publ_section_title
;
 Construction of Larger Molecular Aluminophosphate Cages from the Cyclic
 Four-Ring Building Unit.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3753
_journal_paper_doi               10.1021/ic500083a
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C22 H52 Al2 O6 P2 Si2'
_chemical_formula_weight         584.72
_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                98.789(14)
_cell_angle_beta                 112.477(12)
_cell_angle_gamma                107.401(9)
_cell_formula_units_Z            1
_cell_length_a                   8.5098(10)
_cell_length_b                   10.6686(10)
_cell_length_c                   10.8765(17)
_cell_measurement_reflns_used    7038
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      3.41
_cell_volume                     829.8(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction Ltd, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction Ltd, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6386
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0457
_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)+(0.0713P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                1903
_reflns_number_total             2860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            comp-4_chyba3a.CIF
_cod_data_source_block           t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4337991--4337995.cif.
;
_cod_original_cell_volume        829.76(23)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4337994
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
P1 P 0.35739(11) 0.07022(8) 0.11279(8) 0.0239(2) Uani 1 1 d .
Si1 Si 0.52472(12) 0.37893(9) 0.24326(9) 0.0287(3) Uani 1 1 d .
Al1 Al 0.25959(12) -0.01616(9) -0.21122(9) 0.0247(3) Uani 1 1 d .
O1 O 0.2644(3) 0.0383(2) -0.0443(2) 0.0297(5) Uani 1 1 d .
O2 O 0.5488(3) 0.0690(2) 0.16941(19) 0.0261(5) Uani 1 1 d .
O3 O 0.3702(3) 0.2149(2) 0.1801(2) 0.0306(5) Uani 1 1 d .
C11 C 0.3870(5) 0.4821(3) 0.2509(4) 0.0447(9) Uani 1 1 d .
H11A H 0.2972 0.4695 0.1560 0.067 Uiso 1 1 calc R
H11B H 0.4692 0.5798 0.2958 0.067 Uiso 1 1 calc R
H11C H 0.3216 0.4519 0.3050 0.067 Uiso 1 1 calc R
C12 C 0.7007(5) 0.4015(4) 0.4182(4) 0.0519(10) Uani 1 1 d .
H12A H 0.7724 0.3467 0.4100 0.078 Uiso 1 1 calc R
H12B H 0.6400 0.3708 0.4750 0.078 Uiso 1 1 calc R
H12C H 0.7835 0.4991 0.4628 0.078 Uiso 1 1 calc R
C13 C 0.6260(5) 0.4087(4) 0.1219(4) 0.0409(9) Uani 1 1 d .
H13A H 0.5288 0.3974 0.0306 0.061 Uiso 1 1 calc R
H13B H 0.6817 0.3420 0.1118 0.061 Uiso 1 1 calc R
H13C H 0.7210 0.5024 0.1590 0.061 Uiso 1 1 calc R
C21 C 0.2123(4) -0.0456(3) 0.1646(3) 0.0231(7) Uani 1 1 d .
H21A H 0.1018 -0.0221 0.1463 0.028 Uiso 1 1 calc R
C22 C 0.3105(4) -0.0266(3) 0.3221(3) 0.0266(7) Uani 1 1 d .
H22A H 0.4249 -0.0436 0.3444 0.032 Uiso 1 1 calc R
H22B H 0.3458 0.0698 0.3751 0.032 Uiso 1 1 calc R
C23 C 0.1877(4) -0.1241(3) 0.3673(3) 0.0301(8) Uani 1 1 d .
H23A H 0.2582 -0.1138 0.4672 0.036 Uiso 1 1 calc R
H23B H 0.0807 -0.0995 0.3560 0.036 Uiso 1 1 calc R
C24 C 0.1188(4) -0.2728(3) 0.2815(3) 0.0347(8) Uani 1 1 d .
H24A H 0.0332 -0.3330 0.3091 0.042 Uiso 1 1 calc R
H24B H 0.2249 -0.3006 0.3014 0.042 Uiso 1 1 calc R
C25 C 0.0199(4) -0.2927(3) 0.1260(3) 0.0331(8) Uani 1 1 d .
H25A H -0.0938 -0.2746 0.1046 0.040 Uiso 1 1 calc R
H25B H -0.0171 -0.3895 0.0735 0.040 Uiso 1 1 calc R
C26 C 0.1420(4) -0.1970(3) 0.0787(3) 0.0292(7) Uani 1 1 d .
H26A H 0.0706 -0.2083 -0.0214 0.035 Uiso 1 1 calc R
H26B H 0.2486 -0.2220 0.0900 0.035 Uiso 1 1 calc R
C31 C 0.0293(4) -0.1791(3) -0.3277(3) 0.0330(8) Uani 1 1 d .
H31A H 0.0240 -0.2503 -0.2804 0.050 Uiso 1 1 calc R
H31B H 0.0256 -0.2148 -0.4178 0.050 Uiso 1 1 calc R
H31C H -0.0766 -0.1536 -0.3431 0.050 Uiso 1 1 calc R
C32 C 0.3118(4) 0.1456(3) -0.2772(3) 0.0324(8) Uani 1 1 d .
H32A H 0.4304 0.2179 -0.2072 0.049 Uiso 1 1 calc R
H32B H 0.2134 0.1800 -0.2920 0.049 Uiso 1 1 calc R
H32C H 0.3176 0.1196 -0.3653 0.049 Uiso 1 1 calc R
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'
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
O2 P1 O1 113.06(11) . .
O2 P1 O3 109.09(12) . .
O1 P1 O3 108.63(11) . .
O2 P1 C21 111.59(12) . .
O1 P1 C21 109.68(13) . .
O3 P1 C21 104.39(12) . .
O3 Si1 C12 107.61(15) . .
O3 Si1 C11 104.00(14) . .
C12 Si1 C11 111.73(16) . .
O3 Si1 C13 108.01(14) . .
C12 Si1 C13 111.80(17) . .
C11 Si1 C13 113.16(16) . .
O1 Al1 O2 103.08(9) . 2_655
O1 Al1 C32 108.01(12) . .
O2 Al1 C32 109.03(11) 2_655 .
O1 Al1 C31 107.33(12) . .
O2 Al1 C31 108.66(11) 2_655 .
C32 Al1 C31 119.48(14) . .
P1 O1 Al1 150.40(13) . .
P1 O2 Al1 163.73(14) . 2_655
P1 O3 Si1 137.47(13) . .
C22 C21 C26 110.9(2) . .
C22 C21 P1 111.3(2) . .
C26 C21 P1 112.21(19) . .
C23 C22 C21 111.7(2) . .
C24 C23 C22 111.2(2) . .
C23 C24 C25 111.7(3) . .
C24 C25 C26 111.7(3) . .
C25 C26 C21 110.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O2 1.5106(19) .
P1 O1 1.513(2) .
P1 O3 1.557(2) .
P1 C21 1.789(3) .
Si1 O3 1.682(2) .
Si1 C12 1.840(3) .
Si1 C11 1.847(3) .
Si1 C13 1.849(3) .
Al1 O1 1.801(2) .
Al1 O2 1.801(2) 2_655
Al1 C32 1.963(3) .
Al1 C31 1.965(3) .
O2 Al1 1.801(2) 2_655
C21 C22 1.540(4) .
C21 C26 1.540(4) .
C22 C23 1.521(4) .
C23 C24 1.518(4) .
C24 C25 1.519(4) .
C25 C26 1.524(4) .
