#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/93/4339357.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_4339357
loop_
_publ_author_name
'Gómora-Figueroa, A Paulina'
'Jancik, Vojtech'
'Cea-Olivares, Raymundo'
'Toscano, Rubén A'
_publ_section_title
;
 An unknown coordination mode of the phosphite unit and a carbon-free
 heterocycle in two different heterobimetallic alumophosphites.
;
_journal_issue                   25
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10749
_journal_page_last               10753
_journal_paper_doi               10.1021/ic701614c
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C66 H102 Al2 Li2 N4 O6 P2 S2'
_chemical_formula_sum            'C66 H102 Al2 Li2 N4 O6 P2 S2'
_chemical_formula_weight         1241.42
_chemical_name_systematic
;
 ?
;
_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                 110.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.446(5)
_cell_length_b                   16.854(3)
_cell_length_c                   16.243(3)
_cell_measurement_reflns_used    8084
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.42
_cell_volume                     7023(3)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30949
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.9845
_exptl_absorpt_correction_T_min  0.9497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         6191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0512
_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)+(0.0557P)²+5.3349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                4627
_reflns_number_total             6191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701614c-file008.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 
;
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4339357
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.87312(3) 0.39275(4) 0.01476(5) 0.0404(2) Uani 1 1 d . . .
S1 S 0.78425(3) 0.20071(4) -0.07124(5) 0.03836(19) Uani 1 1 d . . .
Al1 Al 0.84430(3) 0.24654(4) -0.11166(5) 0.02653(18) Uani 1 1 d . . .
O1 O 0.87573(6) 0.33292(9) -0.05681(11) 0.0323(4) Uani 1 1 d . . .
N1 N 0.82702(8) 0.27020(12) -0.23347(13) 0.0294(5) Uani 1 1 d . . .
C1 C 0.93262(11) 0.05963(16) -0.16229(18) 0.0433(7) Uani 1 1 d . . .
H1A H 0.9648 0.0679 -0.1116 0.065 Uiso 1 1 calc R . .
H1B H 0.9411 0.0525 -0.2156 0.065 Uiso 1 1 calc R . .
H1C H 0.9147 0.0122 -0.1525 0.065 Uiso 1 1 calc R . .
Li1 Li 0.78950(19) 0.3076(3) 0.0309(3) 0.0499(12) Uani 1 1 d . . .
O2 O 0.86690(8) 0.33512(12) 0.09257(13) 0.0477(5) Uani 1 1 d . . .
C2 C 0.89758(9) 0.13090(14) -0.17344(16) 0.0309(6) Uani 1 1 d . . .
N2 N 0.89847(7) 0.17295(11) -0.10313(12) 0.0257(4) Uani 1 1 d . . .
O3 O 0.81035(8) 0.41178(11) -0.01367(15) 0.0524(5) Uani 1 1 d . . .
C3 C 0.86519(11) 0.14912(16) -0.25870(17) 0.0368(6) Uani 1 1 d . . .
H3A H 0.8699(10) 0.1189(16) -0.2989(18) 0.044 Uiso 1 1 d . . .
C4 C 0.83598(9) 0.21847(15) -0.28814(16) 0.0323(6) Uani 1 1 d . . .
C5 C 0.81602(11) 0.23293(18) -0.38597(17) 0.0459(7) Uani 1 1 d . . .
H5A H 0.8098 0.2898 -0.3975 0.069 Uiso 0.50 1 calc PR A 1
H5B H 0.7833 0.2039 -0.4136 0.069 Uiso 0.50 1 calc PR A 1
H5C H 0.8419 0.2145 -0.4105 0.069 Uiso 0.50 1 calc PR A 1
H5D H 0.8135 0.1824 -0.4171 0.069 Uiso 0.50 1 d PR A 2
H5E H 0.8401 0.2683 -0.4007 0.069 Uiso 0.50 1 d PR A 2
H5F H 0.7815 0.2576 -0.4040 0.069 Uiso 0.50 1 d PR A 2
C6 C 0.80140(10) 0.34533(15) -0.26924(16) 0.0351(6) Uani 1 1 d . . .
C7 C 0.74700(10) 0.35112(16) -0.29608(17) 0.0383(6) Uani 1 1 d . . .
C8 C 0.72453(12) 0.42443(18) -0.32758(19) 0.0514(8) Uani 1 1 d . . .
H8A H 0.6878 0.4301 -0.3456 0.062 Uiso 1 1 calc R . .
C9 C 0.75392(13) 0.48856(19) -0.3333(2) 0.0592(9) Uani 1 1 d . . .
H9A H 0.7375 0.5377 -0.3555 0.071 Uiso 1 1 calc R . .
C10 C 0.80742(13) 0.48154(18) -0.3068(2) 0.0552(8) Uani 1 1 d . . .
H10A H 0.8276 0.5260 -0.3114 0.066 Uiso 1 1 calc R . .
C11 C 0.83235(11) 0.41001(16) -0.27323(19) 0.0433(7) Uani 1 1 d . . .
C12 C 0.89132(12) 0.40632(19) -0.2447(2) 0.0549(8) Uani 1 1 d . . .
H12A H 0.9028 0.3525 -0.2193 0.066 Uiso 1 1 calc R . .
C13 C 0.90874(13) 0.4174(2) -0.3236(2) 0.0672(10) Uani 1 1 d . . .
H13A H 0.9468 0.4135 -0.3039 0.101 Uiso 1 1 calc R . .
H13B H 0.8976 0.4697 -0.3499 0.101 Uiso 1 1 calc R . .
H13C H 0.8930 0.3761 -0.3674 0.101 Uiso 1 1 calc R . .
C14 C 0.91795(14) 0.4675(2) -0.1745(2) 0.0715(11) Uani 1 1 d . . .
H14A H 0.9097 0.4567 -0.1216 0.107 Uiso 1 1 calc R . .
H14B H 0.9055 0.5207 -0.1967 0.107 Uiso 1 1 calc R . .
H14C H 0.9558 0.4647 -0.1600 0.107 Uiso 1 1 calc R . .
C15 C 0.71216(10) 0.28254(18) -0.29307(18) 0.0431(7) Uani 1 1 d . . .
H15A H 0.7351 0.2373 -0.2628 0.052 Uiso 1 1 calc R . .
C16 C 0.67774(12) 0.3035(2) -0.2396(2) 0.0624(9) Uani 1 1 d . . .
H16A H 0.6997 0.3226 -0.1812 0.094 Uiso 1 1 calc R . .
H16B H 0.6586 0.2562 -0.2333 0.094 Uiso 1 1 calc R . .
H16C H 0.6530 0.3451 -0.2702 0.094 Uiso 1 1 calc R . .
C17 C 0.67796(13) 0.2544(2) -0.3852(2) 0.0601(9) Uani 1 1 d . . .
H17A H 0.7001 0.2403 -0.4188 0.090 Uiso 1 1 calc R . .
H17B H 0.6541 0.2970 -0.4157 0.090 Uiso 1 1 calc R . .
H17C H 0.6578 0.2078 -0.3801 0.090 Uiso 1 1 calc R . .
C18 C 0.94007(9) 0.15927(14) -0.01873(15) 0.0277(5) Uani 1 1 d . . .
C19 C 0.93480(9) 0.10170(14) 0.04007(16) 0.0287(5) Uani 1 1 d . . .
C20 C 0.97531(10) 0.09414(14) 0.12108(16) 0.0340(6) Uani 1 1 d . . .
H20A H 0.9721 0.0565 0.1624 0.041 Uiso 1 1 calc R . .
C21 C 1.01961(10) 0.13939(15) 0.14285(17) 0.0385(6) Uani 1 1 d . . .
H21A H 1.0468 0.1325 0.1983 0.046 Uiso 1 1 calc R . .
C22 C 1.02466(10) 0.19504(15) 0.08397(17) 0.0378(6) Uani 1 1 d . . .
H22A H 1.0556 0.2258 0.0989 0.045 Uiso 1 1 calc R . .
C23 C 0.98490(10) 0.20664(14) 0.00304(16) 0.0319(6) Uani 1 1 d . . .
C24 C 0.99228(10) 0.26891(15) -0.05968(18) 0.0391(6) Uani 1 1 d . . .
H24A H 0.9569 0.2843 -0.1010 0.047 Uiso 1 1 calc R . .
C25 C 1.01879(13) 0.34395(17) -0.0123(2) 0.0562(8) Uani 1 1 d . . .
H25A H 1.0190 0.3841 -0.0557 0.084 Uiso 1 1 calc R . .
H25B H 1.0547 0.3317 0.0254 0.084 Uiso 1 1 calc R . .
H25C H 0.9997 0.3643 0.0241 0.084 Uiso 1 1 calc R . .
C26 C 1.02201(15) 0.2352(2) -0.1147(2) 0.0649(10) Uani 1 1 d . . .
H26A H 1.0036 0.1885 -0.1470 0.097 Uiso 1 1 calc R . .
H26B H 1.0571 0.2198 -0.0760 0.097 Uiso 1 1 calc R . .
H26C H 1.0245 0.2755 -0.1566 0.097 Uiso 1 1 calc R . .
C27 C 0.88848(10) 0.04685(14) 0.02017(17) 0.0355(6) Uani 1 1 d . . .
H27A H 0.8634 0.0592 -0.0403 0.043 Uiso 1 1 calc R . .
C28 C 0.86051(12) 0.05806(18) 0.0853(2) 0.0511(8) Uani 1 1 d . . .
H28A H 0.8479 0.1128 0.0819 0.077 Uiso 1 1 calc R . .
H28B H 0.8847 0.0472 0.1451 0.077 Uiso 1 1 calc R . .
H28C H 0.8309 0.0214 0.0707 0.077 Uiso 1 1 calc R . .
C29 C 0.90520(12) -0.03990(16) 0.0220(2) 0.0523(8) Uani 1 1 d . . .
H29A H 0.9222 -0.0479 -0.0212 0.078 Uiso 1 1 calc R . .
H29B H 0.8745 -0.0742 0.0073 0.078 Uiso 1 1 calc R . .
H29C H 0.9296 -0.0532 0.0809 0.078 Uiso 1 1 calc R . .
C30 C 0.91278(13) 0.29424(18) 0.1481(2) 0.0540(8) Uani 1 1 d . . .
H30A H 0.9393 0.2934 0.1197 0.065 Uiso 1 1 calc R . .
H30B H 0.9039 0.2387 0.1569 0.065 Uiso 1 1 calc R . .
C31 C 0.93425(15) 0.3356(2) 0.2350(2) 0.0675(10) Uani 1 1 d . . .
H31A H 0.9623 0.3036 0.2758 0.101 Uiso 1 1 calc R . .
H31B H 0.9065 0.3427 0.2591 0.101 Uiso 1 1 calc R . .
H31C H 0.9480 0.3875 0.2271 0.101 Uiso 1 1 calc R . .
C32 C 0.78574(14) 0.4649(2) -0.0860(2) 0.0678(10) Uani 1 1 d . . .
H32A H 0.7495 0.4469 -0.1174 0.081 Uiso 1 1 calc R . .
H32B H 0.8045 0.4622 -0.1279 0.081 Uiso 1 1 calc R . .
C33 C 0.78488(18) 0.5467(2) -0.0583(3) 0.0974(15) Uani 1 1 d . . .
H33A H 0.7649 0.5791 -0.1092 0.146 Uiso 1 1 calc R . .
H33B H 0.8206 0.5669 -0.0334 0.146 Uiso 1 1 calc R . .
H33C H 0.7685 0.5493 -0.0136 0.146 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'
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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
O1 P1 O3 103.73(10) . .
O1 P1 O2 103.60(10) . .
O3 P1 O2 86.94(11) . .
O1 P1 Li1 89.71(12) . .
O3 P1 Li1 46.80(13) . .
O2 P1 Li1 46.72(13) . .
Al1 S1 Li1 161.89(13) . 7_655
Al1 S1 Li1 94.45(12) . .
Li1 S1 Li1 72.52(19) 7_655 .
O1 Al1 N2 105.78(9) . .
O1 Al1 N1 104.38(9) . .
N2 Al1 N1 96.41(9) . .
O1 Al1 S1 115.97(7) . .
N2 Al1 S1 114.35(7) . .
N1 Al1 S1 117.57(8) . .
P1 O1 Al1 140.02(11) . .
C4 N1 C6 118.6(2) . .
C4 N1 Al1 121.33(16) . .
C6 N1 Al1 120.00(15) . .
O2 Li1 O3 67.05(17) . .
O2 Li1 S1 136.4(2) . 7_655
O3 Li1 S1 121.7(2) . 7_655
O2 Li1 S1 107.6(2) . .
O3 Li1 S1 110.5(2) . .
S1 Li1 S1 107.48(19) 7_655 .
O2 Li1 P1 35.81(10) . .
O3 Li1 P1 35.78(10) . .
S1 Li1 P1 151.2(2) 7_655 .
S1 Li1 P1 99.71(16) . .
O2 Li1 Li1 149.4(4) . 7_655
O3 Li1 Li1 137.6(4) . 7_655
S1 Li1 Li1 54.99(16) 7_655 7_655
S1 Li1 Li1 52.50(16) . 7_655
P1 Li1 Li1 150.9(3) . 7_655
C30 O2 P1 117.17(18) . .
C30 O2 Li1 136.2(2) . .
P1 O2 Li1 97.47(18) . .
N2 C2 C3 123.1(2) . .
N2 C2 C1 120.1(2) . .
C3 C2 C1 116.8(2) . .
C2 N2 C18 119.35(19) . .
C2 N2 Al1 120.44(16) . .
C18 N2 Al1 120.15(15) . .
C32 O3 P1 119.3(2) . .
C32 O3 Li1 135.2(3) . .
P1 O3 Li1 97.42(18) . .
C2 C3 C4 127.6(2) . .
N1 C4 C3 122.6(2) . .
N1 C4 C5 121.0(2) . .
C3 C4 C5 116.4(2) . .
C11 C6 C7 121.9(2) . .
C11 C6 N1 118.6(2) . .
C7 C6 N1 119.4(2) . .
C8 C7 C6 117.3(3) . .
C8 C7 C15 119.1(2) . .
C6 C7 C15 123.5(2) . .
C9 C8 C7 121.9(3) . .
C8 C9 C10 119.8(3) . .
C9 C10 C11 121.0(3) . .
C10 C11 C6 118.0(3) . .
C10 C11 C12 118.4(3) . .
C6 C11 C12 123.6(2) . .
C11 C12 C14 112.2(3) . .
C11 C12 C13 110.9(3) . .
C14 C12 C13 109.6(3) . .
C7 C15 C17 112.3(2) . .
C7 C15 C16 111.5(2) . .
C17 C15 C16 109.7(2) . .
C23 C18 C19 121.0(2) . .
C23 C18 N2 118.1(2) . .
C19 C18 N2 120.9(2) . .
C20 C19 C18 117.7(2) . .
C20 C19 C27 118.3(2) . .
C18 C19 C27 124.0(2) . .
C21 C20 C19 122.0(2) . .
C20 C21 C22 119.8(2) . .
C21 C22 C23 120.8(2) . .
C22 C23 C18 118.8(2) . .
C22 C23 C24 118.8(2) . .
C18 C23 C24 122.4(2) . .
C26 C24 C25 110.4(2) . .
C26 C24 C23 111.2(2) . .
C25 C24 C23 112.7(2) . .
C19 C27 C28 111.7(2) . .
C19 C27 C29 110.9(2) . .
C28 C27 C29 109.1(2) . .
O2 C30 C31 109.4(2) . .
O3 C32 C33 113.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1 1.5596(17) .
P1 O3 1.649(2) .
P1 O2 1.650(2) .
P1 Li1 2.797(5) .
S1 Al1 2.1244(10) .
S1 Li1 2.343(5) 7_655
S1 Li1 2.419(5) .
Al1 O1 1.7639(18) .
Al1 N2 1.9031(19) .
Al1 N1 1.906(2) .
N1 C4 1.328(3) .
N1 C6 1.465(3) .
C1 C2 1.509(3) .
Li1 O2 2.054(5) .
Li1 O3 2.056(6) .
Li1 S1 2.343(5) 7_655
Li1 Li1 2.817(10) 7_655
O2 C30 1.438(4) .
C2 N2 1.337(3) .
C2 C3 1.388(4) .
N2 C18 1.457(3) .
O3 C32 1.440(4) .
C3 C4 1.402(4) .
C4 C5 1.505(3) .
C6 C11 1.398(4) .
C6 C7 1.402(4) .
C7 C8 1.394(4) .
C7 C15 1.512(4) .
C8 C9 1.372(4) .
C9 C10 1.381(4) .
C10 C11 1.398(4) .
C11 C12 1.518(4) .
C12 C14 1.518(5) .
C12 C13 1.529(4) .
C15 C17 1.532(4) .
C15 C16 1.534(4) .
C18 C23 1.403(3) .
C18 C19 1.405(3) .
C19 C20 1.394(3) .
C19 C27 1.511(3) .
C20 C21 1.371(4) .
C21 C22 1.381(4) .
C22 C23 1.392(4) .
C23 C24 1.526(4) .
C24 C26 1.518(4) .
C24 C25 1.524(4) .
C27 C28 1.523(4) .
C27 C29 1.530(4) .
C30 C31 1.495(4) .
C32 C33 1.454(5) .
