Synthesis and structures of a pentanuclear Al(III) phosphonate cage, an In(III) phosphonate polymer, and coordination compounds of the corresponding phosphonate ester with GaI3 and InCl3.
Richards, Anne F.; Beavers, Christine M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 11305–11310; doi:10.1039/c2dt31280h

data_7020340
_publ_section_title
;
 Synthesis and structures of a pentanuclear Al(III) phosphonate cage, an
 In(III) phosphonate polymer, and coordination compounds of the
 corresponding phosphonate ester with GaI3 and InCl3.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11305
_journal_page_last               11310
_journal_paper_doi               10.1039/c2dt31280h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C17 H24 Cl3 In N O6 P'
_chemical_formula_sum            'C17 H24 Cl3 In N O6 P'
_chemical_formula_weight         590.51
_chemical_name_systematic
;
?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2012-06-06
_audit_creation_method
;
Olex2 1.1
(compiled Nov 1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                99.131(4)
_cell_angle_beta                 92.125(3)
_cell_angle_gamma                117.475(4)
_cell_formula_units_Z            2
_cell_length_a                   7.9265(3)
_cell_length_b                   8.0262(3)
_cell_length_c                   21.3673(9)
_cell_measurement_reflns_used    8670
_cell_measurement_temperature    173.2
_cell_measurement_theta_max      30.8700
_cell_measurement_theta_min      2.4553
_cell_volume                     1181.30(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.2
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
1 omega -25.00 47.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 15.0885 -99.0000 67.0000 72

2 omega -19.00 94.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 15.0885 77.0000 -180.0000 113

3 omega -25.00 0.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -15.8697 -99.0000 6.0000 25

4 omega -64.00 49.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 15.0885 -77.0000 -150.0000 113

5 omega -19.00 94.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 15.0885 77.0000 -60.0000 113

6 omega -58.00 4.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -15.8697 99.0000 -67.0000 62
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0426286000
_diffrn_orient_matrix_UB_12      -0.0520158000
_diffrn_orient_matrix_UB_13      -0.0163458000
_diffrn_orient_matrix_UB_21      -0.0666111000
_diffrn_orient_matrix_UB_22      -0.0271590000
_diffrn_orient_matrix_UB_23      -0.0275615000
_diffrn_orient_matrix_UB_31      0.0638912000
_diffrn_orient_matrix_UB_32      0.0829718000
_diffrn_orient_matrix_UB_33      -0.0110390000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15037
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug 2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0367
_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/[\s^2^(Fo^2^)+(0.0306P)^2^+1.3222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                4778
_reflns_number_total             5421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31280h.txt
_cod_data_source_block           ar42
_cod_original_cell_volume        1181.30(8)
_cod_database_code               7020340
_chemical_oxdiff_formula         'C12 H12 N1 P1 O1 IN1 CL1'
_chemical_oxdiff_usercomment     'PHTAL INCL3 THF'
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22