#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/39/4323916.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_4323916
loop_
_publ_author_name
'Mark R. Mason'
'R. Mark Matthews'
'Mark S. Mashuta'
'John F. Richardson'
_publ_contact_author
;
Mark R. Mason
Department of Chemistry and Center for Chemical Catalysis
University of Louisville
Louisville
KY 40292
USA
;
_publ_contact_author_email       ' MRMASO01@homer.lousiville.edu '
_publ_contact_author_fax         (502)852-8149
_publ_contact_author_phone       '(502)852-6612 '
_publ_section_title
;
 Organic-Soluble Cyclic and Cage Alkylaluminophosphates: X-ray Crystal
 Structure of [(tBu)2Al(μ2-O)2P(OSiMe3)2]2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5756
_journal_page_last               5757
_journal_paper_doi               10.1021/ic960619v
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         'C28 H72 Al2 O8 P2 Si4 '
_chemical_formula_sum            'C28 H72 Al2 O8 P2 Si4'
_chemical_formula_weight         765.12
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             'Wed Jun 12 03:18:35 1996'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 118.26(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.040(12)
_cell_length_b                   12.778(9)
_cell_length_c                   20.298(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      30.0
_cell_volume                     4807(6)
_computing_cell_refinement       'Enraf Nonius Diffractometer Control'
_computing_data_collection       'Enraf Nonius Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_orient_matrix_UB_11      0.03040
_diffrn_orient_matrix_UB_12      0.05133
_diffrn_orient_matrix_UB_13      0.03968
_diffrn_orient_matrix_UB_21      0.02419
_diffrn_orient_matrix_UB_22      -0.05895
_diffrn_orient_matrix_UB_23      0.03555
_diffrn_orient_matrix_UB_31      0.03745
_diffrn_orient_matrix_UB_32      -0.00375
_diffrn_orient_matrix_UB_33      -0.01701
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4564
_diffrn_reflns_theta_max         24.97
_diffrn_standards_decay_%        -13.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.62
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_description       block
_exptl_crystal_F_000             1664.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.24
_refine_ls_goodness_of_fit_obs   1.712
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2007
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.054
_refine_ls_shift/esd_max         0.0180
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/σ²(F)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.055
_reflns_number_observed          2007
_reflns_number_total             4490
_reflns_observed_criterion       I>3\s(I)
_cod_data_source_file            ic960619v.cif
_cod_data_source_block           COMPOUND#1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w=1/\s^2^(F)' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/\s^2^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4806(5)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C28 H72 Al2 O8 P2 Si4 '
_cod_database_code               4323916
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2+x,1/2+y,   +z'
'   -x,   +y,1/2-z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
'1/2-x,1/2-y,   -z'
'   +x,   -y,1/2+z'
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
P(1) 0.77304(7) -0.2359(1) -0.09475(7) 0.0426(4) Uij ? ?
Si(1) 0.91530(9) -0.2076(1) -0.09776(10) 0.0658(6) Uij ? ?
Si(2) 0.66626(9) -0.2165(2) -0.26317(9) 0.0729(6) Uij ? ?
Al(1) 0.7468(1) -0.4306(1) -0.01039(10) 0.0599(6) Uij ? ?
O(1) 0.7532(2) -0.3328(3) -0.0700(2) 0.083(2) Uij ? ?
O(2) 0.7805(2) -0.1450(3) -0.0472(2) 0.073(1) Uij ? ?
O(3) 0.8421(2) -0.2547(3) -0.0984(2) 0.090(2) Uij ? ?
O(4) 0.7177(2) -0.2092(4) -0.1731(2) 0.114(2) Uij ? ?
C(1) 0.8436(4) -0.4900(6) 0.0527(4) 0.091(3) Uij ? ?
C(2) 0.8709(5) -0.5467(8) 0.0047(5) 0.179(4) Uij ? ?
C(3) 0.8975(4) -0.4041(8) 0.0953(4) 0.138(4) Uij ? ?
C(4) 0.8439(5) -0.5663(7) 0.1100(5) 0.156(4) Uij ? ?
C(5) 0.6646(4) -0.5204(5) -0.0752(4) 0.081(2) Uij ? ?
C(6) 0.6735(5) -0.5664(8) -0.1392(5) 0.167(4) Uij ? ?
C(7) 0.5958(4) -0.4567(7) -0.1093(5) 0.141(4) Uij ? ?
C(8) 0.6533(5) -0.6102(7) -0.0321(5) 0.157(4) Uij ? ?
C(9) 0.9292(4) -0.2839(6) -0.1655(4) 0.118(3) Uij ? ?
C(10) 0.8988(4) -0.0698(6) -0.1256(5) 0.139(4) Uij ? ?
C(11) 0.9892(4) -0.2230(7) -0.0045(4) 0.123(3) Uij ? ?
C(12) 0.7092(4) -0.2950(7) -0.3053(4) 0.127(3) Uij ? ?
C(13) 0.6567(6) -0.0848(7) -0.2961(5) 0.185(5) Uij ? ?
C(14) 0.5818(4) -0.2730(9) -0.2782(4) 0.158(4) Uij ? ?
H(2a) 0.8404 -0.6059 -0.0191 0.2140 Uij ? ?
H(2b) 0.8746 -0.5035 -0.0288 0.2140 Uij ? ?
H(2c) 0.9201 -0.5795 0.0362 0.2140 Uij ? ?
H(3a) 0.9468 -0.4337 0.1275 0.1634 Uij ? ?
H(3b) 0.9010 -0.3582 0.0622 0.1634 Uij ? ?
H(3c) 0.8841 -0.3708 0.1283 0.1634 Uij ? ?
H(4a) 0.8274 -0.5347 0.1413 0.1925 Uij ? ?
H(4b) 0.8082 -0.6227 0.0822 0.1925 Uij ? ?
H(4c) 0.8881 -0.6024 0.1402 0.1925 Uij ? ?
H(6a) 0.6345 -0.6082 -0.1719 0.2014 Uij ? ?
H(6b) 0.6807 -0.5112 -0.1672 0.2014 Uij ? ?
H(6c) 0.7167 -0.6081 -0.1174 0.2014 Uij ? ?
H(7a) 0.5871 -0.4277 -0.0696 0.1684 Uij ? ?
H(7b) 0.5986 -0.3986 -0.1374 0.1684 Uij ? ?
H(7c) 0.5534 -0.4964 -0.1412 0.1684 Uij ? ?
H(8a) 0.6436 -0.5809 0.0058 0.1887 Uij ? ?
H(8b) 0.6101 -0.6504 -0.0654 0.1887 Uij ? ?
H(8c) 0.6927 -0.6522 -0.0129 0.1887 Uij ? ?
H(9a) 0.9312 -0.3594 -0.1545 0.1418 Uij ? ?
H(9b) 0.8848 -0.2797 -0.2163 0.1418 Uij ? ?
H(9c) 0.9678 -0.2658 -0.1718 0.1418 Uij ? ?
H(10a) 0.9361 -0.0339 -0.1277 0.1672 Uij ? ?
H(10b) 0.8552 -0.0614 -0.1766 0.1672 Uij ? ?
H(10c) 0.8839 -0.0283 -0.0937 0.1672 Uij ? ?
H(11a) 0.9979 -0.2949 0.0127 0.1456 Uij ? ?
H(11b) 1.0346 -0.1953 0.0028 0.1456 Uij ? ?
H(11c) 0.9801 -0.1860 0.0339 0.1456 Uij ? ?
H(12a) 0.7190 -0.3671 -0.2821 0.1811 Uij ? ?
H(12b) 0.6825 -0.3039 -0.3561 0.1811 Uij ? ?
H(12c) 0.7569 -0.2691 -0.2923 0.1811 Uij ? ?
H(13a) 0.6983 -0.0493 -0.2852 0.2204 Uij ? ?
H(13b) 0.6234 -0.0789 -0.3505 0.2204 Uij ? ?
H(13c) 0.6300 -0.0406 -0.2749 0.2204 Uij ? ?
H(14a) 0.5569 -0.2329 -0.2576 0.1900 Uij ? ?
H(14b) 0.5469 -0.2813 -0.3321 0.1900 Uij ? ?
H(14c) 0.5873 -0.3435 -0.2580 0.1900 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 112 0.003 0.002 'International Tables'
H 0 288 0.000 0.000 'International Tables'
Al 0 8 0.064 0.051 'International Tables'
P 0 8 0.102 0.094 'International Tables'
Si 0 16 0.082 0.070 'International Tables'
O 0 32 0.011 0.006 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) P(1) O(2) 113.6(2) ? ? ? yes
O(1) P(1) O(3) 108.7(2) ? ? ? no
O(1) P(1) O(4) 110.6(3) ? ? ? no
O(2) P(1) O(3) 110.5(2) ? ? ? no
O(2) P(1) O(4) 107.7(3) ? ? ? no
O(3) P(1) O(4) 105.4(3) ? ? ? no
O(3) Si(1) C(9) 106.4(3) ? ? ? no
O(3) Si(1) C(10) 108.1(3) ? ? ? no
O(3) Si(1) C(11) 107.9(3) ? ? ? no
C(9) Si(1) C(10) 110.9(4) ? ? ? no
C(9) Si(1) C(11) 111.5(4) ? ? ? no
C(10) Si(1) C(11) 111.8(4) ? ? ? no
O(4) Si(2) C(12) 110.3(3) ? ? ? no
O(4) Si(2) C(13) 105.2(4) ? ? ? no
O(4) Si(2) C(14) 106.9(3) ? ? ? no
C(12) Si(2) C(13) 109.7(4) ? ? ? no
C(12) Si(2) C(14) 111.7(4) ? ? ? no
C(13) Si(2) C(14) 112.8(5) ? ? ? no
O(1) Al(1) O(2) 102.3(2) ? ? ? yes
O(1) Al(1) C(1) 108.8(3) ? ? ? no
O(1) Al(1) C(5) 106.2(3) ? ? ? no
O(2) Al(1) C(1) 109.4(2) ? ? ? no
O(2) Al(1) C(5) 107.1(2) ? ? ? no
C(1) Al(1) C(5) 121.3(3) ? ? ? no
P(1) O(1) Al(1) 160.9(3) ? ? ? yes
P(1) O(2) Al(1) 151.4(2) ? ? ? yes
P(1) O(3) Si(1) 149.2(3) ? ? ? no
P(1) O(4) Si(2) 161.4(4) ? ? ? no
Al(1) C(1) C(2) 110.6(5) ? ? ? no
Al(1) C(1) C(3) 110.7(5) ? ? ? no
Al(1) C(1) C(4) 111.9(5) ? ? ? no
C(2) C(1) C(3) 107.5(7) ? ? ? no
C(2) C(1) C(4) 108.6(7) ? ? ? no
C(3) C(1) C(4) 107.4(7) ? ? ? no
Al(1) C(5) C(6) 111.8(5) ? ? ? no
Al(1) C(5) C(7) 109.9(5) ? ? ? no
Al(1) C(5) C(8) 112.4(5) ? ? ? no
C(6) C(5) C(7) 107.2(7) ? ? ? no
C(6) C(5) C(8) 108.4(7) ? ? ? no
C(7) C(5) C(8) 106.9(6) ? ? ? no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P(1) O(1) 1.471(4) ? ? yes
P(1) O(2) 1.469(4) ? ? yes
P(1) O(3) 1.508(4) ? ? no
P(1) O(4) 1.499(4) ? ? no
Si(1) O(3) 1.650(4) ? ? no
Si(1) C(9) 1.816(7) ? ? no
Si(1) C(10) 1.832(8) ? ? no
Si(1) C(11) 1.804(7) ? ? no
Si(2) O(4) 1.628(4) ? ? no
Si(2) C(12) 1.810(7) ? ? no
Si(2) C(13) 1.787(9) ? ? no
Si(2) C(14) 1.807(8) ? ? no
Al(1) O(1) 1.790(4) ? ? yes
Al(1) O(2) 1.805(4) ? ? yes
Al(1) C(1) 1.972(7) ? ? no
Al(1) C(5) 1.972(6) ? ? no
C(1) C(2) 1.524(9) ? ? no
C(1) C(3) 1.520(10) ? ? no
C(1) C(4) 1.517(10) ? ? no
C(5) C(6) 1.515(9) ? ? no
C(5) C(7) 1.511(10) ? ? no
C(5) C(8) 1.531(9) ? ? no
