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_4332040
_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            'C115 H169 Al3 Br N6 O15 P2'
_chemical_formula_weight         2098.35
_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                89.9924(4)
_cell_angle_beta                 71.8021(4)
_cell_angle_gamma                82.2916(4)
_cell_formula_units_Z            2
_cell_length_a                   15.02320(10)
_cell_length_b                   18.8031(2)
_cell_length_c                   21.9993(3)
_cell_measurement_reflns_used    21356
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.00
_cell_volume                     5844.49(11)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN, Nonius, 1998'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1995)'
_computing_publication_material
;
SHELXL97-2 (sheldrick, 1997) and local procedures)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius Kappa CCD 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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.1047
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41073
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.9551
_exptl_absorpt_correction_T_min  0.8546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2250
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1311
_refine_ls_number_reflns         20590
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+2.5757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2158
_reflns_number_gt                11540
_reflns_number_total             20590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic052090ksup2.cif
_cod_data_source_block           k05067
_cod_database_code               4332040