A hexacoordinated aluminium complex with a new type of seven-membered chelate ring involving a cyclic phosphate ester
Satish Kumar, N.; Vittal, Jagadese J.; Kumara Swamy, K. C.; Acta Crystallographica Section E 60 (2004) m1321–m1323; doi:10.1107/S1600536804019592

data_2204190
_publ_section_title
;
 A hexacoordinated aluminium complex with a new type of seven-membered
 chelate ring involving a cyclic phosphate ester
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1321
_journal_page_last               m1323
_journal_paper_doi               10.1107/S1600536804019592
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Al (C29 H30 Cl4 O5 P)3] , 0.25C6 H6'
_chemical_formula_moiety         'C87 H90 Al Cl12 O15 P3 , 0.25C6 H6'
_chemical_formula_sum            'C88.5 H91.5 Al Cl12 O15 P3'
_chemical_formula_weight         1940.41
_chemical_name_systematic
;
[tris(2,3,4,5-tetrachloro-6-(4,8-di-tert-butyl-2,10-
dimethyl-6-oxo-12H-5,7-dioxa-6\l^5^-phosphadibenzo[a,d]cycloocten-6-
yloxy)phenoxido]aluminium benzene 0.25-solvate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.4062(7)
_cell_length_b                   22.4062(7)
_cell_length_c                   33.854(2)
_cell_measurement_reflns_used    8257
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.4
_cell_measurement_theta_min      2.65
_cell_volume                     14719.0(11)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEX-6a (McArdle, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.333
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28911
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.8313
_exptl_absorpt_correction_T_min  0.6325
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       cube
_exptl_crystal_F_000             6027
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5770
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0581
_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/[\s^2^(Fo^2^)+(0.09P)^2^+7.037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                4591
_reflns_number_total             5770
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6086.cif
_cod_data_source_block           II
_cod_original_cell_volume        14718.8(12)
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C88.5 H91.5 Al1 Cl12 O15 P3'
_cod_database_code               2204190
_cod_database_fobs_code          2204190