Ligand-Tetrahydrofuran Coupling in Chelated Aluminum Phosphinates
Y. Wang; S. Parkin; D. Atwood; Inorganic Chemistry 41 (2002) 558–565; doi:10.1021/ic0110326

data_4317522
_publ_section_title
;
 Ligand-Tetrahydrofuran Coupling in Chelated Aluminum Phosphinates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              558
_journal_page_last               565
_journal_paper_doi               10.1021/ic0110326
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C57 H67.5 Al N2 O5 P'
_chemical_formula_weight         918.58
_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                109.56(3)
_cell_angle_beta                 96.48(3)
_cell_angle_gamma                93.56(3)
_cell_formula_units_Z            2
_cell_length_a                   13.214(5)
_cell_length_b                   13.480(5)
_cell_length_c                   15.347(5)
_cell_measurement_reflns_used    56148
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.0
_cell_volume                     2544.9(17)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material
'SHELX97-2 (Sheldrick, 1997) and local procedures'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.1122
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10708
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             983
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         .790
_refine_diff_density_min         -.515
_refine_diff_density_rms         .097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         5473
_refine_ls_number_restraints     1025
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1522
_refine_ls_R_factor_gt           0.1112
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1665P)^2^+7.0385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3087
_refine_ls_wR_factor_ref         0.3314
_reflns_number_gt                3895
_reflns_number_total             5473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110326_6.cif
_cod_data_source_block
k00150_[Salomphen(thf)(tBu)AlO2P(H)Ph]2_Compound14
_cod_original_cell_volume        2544.8(16)
_cod_original_formula_sum        'C57 H67.50 Al N2 O5 P'
_cod_database_code               4317522