Aluminum Phosphinate and Phosphates of Salen Ligands
Mitra, Amitabha; Parkin, Sean; Atwood, David A.; Inorganic Chemistry 45 (2006) 3970–3975; doi:10.1021/ic052090k

data_4332039
_publ_section_title
;
 Aluminum Phosphinate and Phosphates of Salen Ligands
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3970
_journal_page_last               3975
_journal_paper_doi               10.1021/ic052090k
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C45 H60 Al N2 O5 P'
_chemical_formula_weight         766.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.6850(2)
_cell_length_b                   26.1840(5)
_cell_length_c                   28.1148(5)
_cell_measurement_reflns_used    7431
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.23
_cell_measurement_theta_min      1.00
_cell_volume                     8602.0(3)
_computing_cell_refinement       'APEX2 (Bruker-Nonius, 2004)'
_computing_data_collection       'APEX2 (Bruker-Nonius, 2004)'
_computing_data_reduction        'APEX2 (Bruker-Nonius, 2004)'
_computing_molecular_graphics    'XP in 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      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full .991
_diffrn_measured_fraction_theta_max .991
_diffrn_measurement_device_type  'Bruker-Nonius X8 Proteum'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'graded multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48842
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  0.8962
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS in APEX2 (Bruker-Nonius, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'broken fragment'
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         .415
_refine_diff_density_min         -.277
_refine_diff_density_rms         .048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.484(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         15283
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+2.8631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                14037
_reflns_number_total             15283
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic052090ksup1.cif
_cod_data_source_block           x05016
_cod_database_code               4332039