#------------------------------------------------------------------------------
#$Date: 2018-08-21 22:46:58 +0300 (Tue, 21 Aug 2018) $
#$Revision: 210021 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/86/4338634.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4338634
loop_
_publ_author_name
'Lee, Pei-Ying'
'Liang, Lan-Chang'
_publ_section_title
;
 Synthesis and Structural Characterization of Five-Coordinate Aluminum
 Complexes Containing Diarylamido Diphosphine Ligands
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5480
_journal_page_last               5487
_journal_paper_doi               10.1021/ic802030d
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C24 H36 Al Cl2 N P2'
_chemical_formula_sum            'C24 H36 Al Cl2 N P2'
_chemical_formula_weight         498.36
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ya'
_symmetry_space_group_name_H-M   'P 1 2/a 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                 116.8740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2082(4)
_cell_length_b                   9.2626(3)
_cell_length_c                   18.4636(6)
_cell_measurement_reflns_used    15219
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     2625.13(14)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0816
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16573
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_correction_T_min  0.8332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.263
_refine_ls_extinction_coef       0.048(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.1111
_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/[σ²(Fo²)+(0.1268P)²+17.9642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3116
_refine_ls_wR_factor_ref         0.3355
_reflns_number_gt                3684
_reflns_number_total             4770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802030d_si_001.cif
_cod_data_source_block           6406_5b
_cod_original_sg_symbol_H-M      'P 2/a'
_cod_database_code               4338634
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'-x, -y, -z'
'x-1/2, -y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cl1 Cl 0.23170(13) 0.0171(2) 0.08941(13) 0.0480(6) Uani 1 1 d .
Cl2 Cl 0.14113(17) 0.5033(3) 0.41169(16) 0.0611(8) Uani 1 1 d .
P1 P 0.40811(13) 0.1966(2) 0.08264(12) 0.0338(6) Uani 1 1 d .
P2 P 0.32236(14) 0.6801(2) 0.41174(13) 0.0366(6) Uani 1 1 d .
Al1 Al 0.2500 0.1509(4) 0.0000 0.0349(8) Uani 1 2 d S
Al2 Al 0.2500 0.6327(4) 0.5000 0.0392(9) Uani 1 2 d S
N1 N 0.2500 0.3595(10) 0.0000 0.038(2) Uani 1 2 d S
N2 N 0.2500 0.8396(10) 0.5000 0.037(2) Uani 1 2 d S
C1 C 0.4832(6) 0.0956(9) 0.1741(5) 0.0418(19) Uani 1 1 d .
H1 H 0.5400 0.1439 0.1971 0.050 Uiso 1 1 calc R
C2 C 0.4508(7) 0.0906(13) 0.2401(6) 0.059(3) Uani 1 1 d .
H2A H 0.4445 0.1873 0.2556 0.089 Uiso 1 1 calc R
H2B H 0.4923 0.0393 0.2868 0.089 Uiso 1 1 calc R
H2C H 0.3955 0.0423 0.2188 0.089 Uiso 1 1 calc R
C3 C 0.4943(7) -0.0556(11) 0.1477(6) 0.061(3) Uani 1 1 d .
H3A H 0.5142 -0.0490 0.1069 0.091 Uiso 1 1 calc R
H3B H 0.4394 -0.1052 0.1259 0.091 Uiso 1 1 calc R
H3C H 0.5362 -0.1078 0.1936 0.091 Uiso 1 1 calc R
C4 C 0.4657(5) 0.2167(9) 0.0186(5) 0.0407(19) Uani 1 1 d .
H4 H 0.4645 0.1222 -0.0058 0.049 Uiso 1 1 calc R
C5 C 0.4170(7) 0.3204(11) -0.0499(6) 0.053(2) Uani 1 1 d .
H5A H 0.3574 0.2904 -0.0791 0.080 Uiso 1 1 calc R
H5B H 0.4433 0.3215 -0.0861 0.080 Uiso 1 1 calc R
H5C H 0.4195 0.4155 -0.0283 0.080 Uiso 1 1 calc R
C6 C 0.5609(6) 0.2599(12) 0.0666(7) 0.056(3) Uani 1 1 d .
H6A H 0.5904 0.1911 0.1092 0.084 Uiso 1 1 calc R
H6B H 0.5645 0.3539 0.0897 0.084 Uiso 1 1 calc R
H6C H 0.5879 0.2618 0.0310 0.084 Uiso 1 1 calc R
C7 C 0.3955(5) 0.3759(9) 0.1140(5) 0.0376(18) Uani 1 1 d .
C8 C 0.4587(6) 0.4499(10) 0.1811(6) 0.046(2) Uani 1 1 d .
H8 H 0.5125 0.4071 0.2124 0.055 Uiso 1 1 calc R
C9 C 0.4415(6) 0.5848(9) 0.2009(6) 0.048(2) Uani 1 1 d .
H9 H 0.4842 0.6354 0.2441 0.057 Uiso 1 1 calc R
C10 C 0.3591(6) 0.6451(10) 0.1553(6) 0.048(2) Uani 1 1 d .
H10 H 0.3468 0.7355 0.1695 0.057 Uiso 1 1 calc R
C11 C 0.2962(6) 0.5745(9) 0.0906(5) 0.0406(19) Uani 1 1 d .
H11 H 0.2417 0.6168 0.0618 0.049 Uiso 1 1 calc R
C12 C 0.3128(5) 0.4386(9) 0.0667(5) 0.0356(18) Uani 1 1 d .
C13 C 0.3079(6) 0.5793(10) 0.3205(5) 0.046(2) Uani 1 1 d .
H13 H 0.3348 0.6360 0.2930 0.056 Uiso 1 1 calc R
C14 C 0.2119(6) 0.5585(12) 0.2606(5) 0.054(2) Uani 1 1 d .
H14A H 0.1833 0.6506 0.2476 0.081 Uiso 1 1 calc R
H14B H 0.1846 0.4977 0.2845 0.081 Uiso 1 1 calc R
H14C H 0.2076 0.5141 0.2119 0.081 Uiso 1 1 calc R
C15 C 0.3549(7) 0.4347(11) 0.3437(6) 0.060(3) Uani 1 1 d .
H15A H 0.4151 0.4503 0.3809 0.090 Uiso 1 1 calc R
H15B H 0.3509 0.3875 0.2958 0.090 Uiso 1 1 calc R
H15C H 0.3285 0.3751 0.3690 0.090 Uiso 1 1 calc R
C16 C 0.4419(5) 0.7167(10) 0.4680(5) 0.044(2) Uani 1 1 d .
H16 H 0.4707 0.6246 0.4906 0.052 Uiso 1 1 calc R
C17 C 0.4615(6) 0.8175(10) 0.5388(6) 0.053(2) Uani 1 1 d .
H17A H 0.4370 0.7789 0.5722 0.079 Uiso 1 1 calc R
H17B H 0.4365 0.9106 0.5187 0.079 Uiso 1 1 calc R
H17C H 0.5234 0.8270 0.5704 0.079 Uiso 1 1 calc R
C18 C 0.4806(7) 0.7742(14) 0.4138(7) 0.069(3) Uani 1 1 d .
H18A H 0.4683 0.7078 0.3700 0.103 Uiso 1 1 calc R
H18B H 0.5425 0.7846 0.4451 0.103 Uiso 1 1 calc R
H18C H 0.4552 0.8664 0.3921 0.103 Uiso 1 1 calc R
C19 C 0.2730(5) 0.8560(9) 0.3794(5) 0.0378(18) Uani 1 1 d .
C20 C 0.2640(6) 0.9279(10) 0.3104(5) 0.047(2) Uani 1 1 d .
H20 H 0.2839 0.8850 0.2764 0.056 Uiso 1 1 calc R
C21 C 0.2256(7) 1.0635(11) 0.2915(6) 0.057(3) Uani 1 1 d .
H21 H 0.2216 1.1131 0.2462 0.068 Uiso 1 1 calc R
C22 C 0.1935(6) 1.1235(10) 0.3410(6) 0.053(2) Uani 1 1 d .
H22 H 0.1670 1.2137 0.3284 0.063 Uiso 1 1 calc R
C23 C 0.2003(6) 1.0515(9) 0.4089(6) 0.044(2) Uani 1 1 d .
H23 H 0.1774 1.0931 0.4409 0.053 Uiso 1 1 calc R
C24 C 0.2416(5) 0.9157(8) 0.4307(5) 0.0351(18) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C7 P1 C1 108.0(4) . .
C7 P1 C4 106.7(4) . .
C1 P1 C4 106.1(4) . .
C7 P1 Al1 95.6(3) . .
C1 P1 Al1 126.5(3) . .
C4 P1 Al1 112.1(3) . .
C19 P2 C13 107.8(4) . .
C19 P2 C16 104.8(4) . .
C13 P2 C16 105.1(4) . .
C19 P2 Al2 94.3(3) . .
C13 P2 Al2 127.3(3) . .
C16 P2 Al2 114.7(3) . .
N1 Al1 Cl1 124.34(10) . .
N1 Al1 Cl1 124.34(10) . 2
Cl1 Al1 Cl1 111.32(19) . 2
N1 Al1 P1 80.18(9) . .
Cl1 Al1 P1 97.12(8) . .
Cl1 Al1 P1 93.93(8) 2 .
N1 Al1 P1 80.18(9) . 2
Cl1 Al1 P1 93.93(8) . 2
Cl1 Al1 P1 97.12(8) 2 2
P1 Al1 P1 160.36(18) . 2
N2 Al2 Cl2 123.00(11) . .
N2 Al2 Cl2 123.00(11) . 2_556
Cl2 Al2 Cl2 114.0(2) . 2_556
N2 Al2 P2 79.86(9) . .
Cl2 Al2 P2 96.95(8) . .
Cl2 Al2 P2 94.05(8) 2_556 .
N2 Al2 P2 79.86(9) . 2_556
Cl2 Al2 P2 94.05(8) . 2_556
Cl2 Al2 P2 96.95(8) 2_556 2_556
P2 Al2 P2 159.72(18) . 2_556
C12 N1 C12 117.9(9) . 2
C12 N1 Al1 121.0(4) . .
C12 N1 Al1 121.0(4) 2 .
C24 N2 C24 120.0(9) 2_556 .
C24 N2 Al2 120.0(5) 2_556 .
C24 N2 Al2 120.0(5) . .
C3 C1 C2 111.4(8) . .
C3 C1 P1 108.1(6) . .
C2 C1 P1 112.3(6) . .
C3 C1 H1 108.3 . .
C2 C1 H1 108.3 . .
P1 C1 H1 108.3 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C4 C6 111.4(8) . .
C5 C4 P1 110.1(6) . .
C6 C4 P1 113.5(6) . .
C5 C4 H4 107.2 . .
C6 C4 H4 107.2 . .
P1 C4 H4 107.2 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C8 C7 C12 120.4(8) . .
C8 C7 P1 125.1(7) . .
C12 C7 P1 114.4(6) . .
C9 C8 C7 120.4(9) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 C10 119.1(8) . .
C8 C9 H9 120.5 . .
C10 C9 H9 120.5 . .
C11 C10 C9 121.6(8) . .
C11 C10 H10 119.2 . .
C9 C10 H10 119.2 . .
C10 C11 C12 120.8(8) . .
C10 C11 H11 119.6 . .
C12 C11 H11 119.6 . .
C11 C12 C7 117.7(7) . .
C11 C12 N1 123.4(7) . .
C7 C12 N1 118.8(7) . .
C15 C13 C14 110.9(8) . .
C15 C13 P2 110.7(7) . .
C14 C13 P2 112.4(6) . .
C15 C13 H13 107.5 . .
C14 C13 H13 107.5 . .
P2 C13 H13 107.5 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C13 C15 H15A 109.5 . .
C13 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C13 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C17 C16 C18 110.9(8) . .
C17 C16 P2 110.6(6) . .
C18 C16 P2 113.3(7) . .
C17 C16 H16 107.3 . .
C18 C16 H16 107.3 . .
P2 C16 H16 107.3 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C16 C18 H18A 109.5 . .
C16 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C16 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C20 C19 C24 121.1(8) . .
C20 C19 P2 125.3(7) . .
C24 C19 P2 113.6(6) . .
C19 C20 C21 120.7(9) . .
C19 C20 H20 119.7 . .
C21 C20 H20 119.7 . .
C22 C21 C20 119.0(9) . .
C22 C21 H21 120.5 . .
C20 C21 H21 120.5 . .
C23 C22 C21 120.8(9) . .
C23 C22 H22 119.6 . .
C21 C22 H22 119.6 . .
C22 C23 C24 121.1(8) . .
C22 C23 H23 119.5 . .
C24 C23 H23 119.5 . .
C19 C24 C23 117.3(7) . .
C19 C24 N2 120.3(7) . .
C23 C24 N2 122.4(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 Al1 2.198(3) .
Cl2 Al2 2.201(3) .
P1 C7 1.803(8) .
P1 C1 1.850(9) .
P1 C4 1.863(8) .
P1 Al1 2.481(2) .
P2 C19 1.809(8) .
P2 C13 1.842(9) .
P2 C16 1.869(9) .
P2 Al2 2.497(2) .
Al1 N1 1.932(10) .
Al1 Cl1 2.198(3) 2
Al1 P1 2.481(2) 2
Al2 N2 1.916(10) .
Al2 Cl2 2.201(3) 2_556
Al2 P2 2.497(2) 2_556
N1 C12 1.420(9) .
N1 C12 1.420(9) 2
N2 C24 1.410(9) 2_556
N2 C24 1.410(9) .
C1 C3 1.523(13) .
C1 C2 1.555(13) .
C1 H1 0.9800 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 C5 1.506(13) .
C4 C6 1.523(13) .
C4 H4 0.9800 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.403(12) .
C7 C12 1.415(11) .
C8 C9 1.371(12) .
C8 H8 0.9300 .
C9 C10 1.398(13) .
C9 H9 0.9300 .
C10 C11 1.363(12) .
C10 H10 0.9300 .
C11 C12 1.405(11) .
C11 H11 0.9300 .
C13 C15 1.523(13) .
C13 C14 1.528(12) .
C13 H13 0.9800 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 C17 1.516(12) .
C16 C18 1.527(14) .
C16 H16 0.9800 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 C20 1.382(12) .
C19 C24 1.399(11) .
C20 C21 1.388(13) .
C20 H20 0.9300 .
C21 C22 1.381(14) .
C21 H21 0.9300 .
C22 C23 1.377(13) .
C22 H22 0.9300 .
C23 C24 1.410(11) .
C23 H23 0.9300 .
