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

data_4317517
_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            'C48 H69 Al N2 O3'
_chemical_formula_weight         749.03
_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                 119.965(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.539(6)
_cell_length_b                   10.2870(15)
_cell_length_c                   27.986(5)
_cell_measurement_reflns_used    55784
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.00
_cell_volume                     8864(3)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5782
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.32
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.25
_refine_diff_density_max         .902
_refine_diff_density_min         -.617
_refine_diff_density_rms         .068
_refine_ls_extinction_coef       0.00041(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         5782
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+43.7324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2195
_reflns_number_gt                4498
_reflns_number_total             5782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110326_1.cif
_cod_data_source_block           k01072m_Salomphen(tBu)AlMe_Compound5
_cod_original_cell_volume        8864(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4317517