#------------------------------------------------------------------------------
#$Date: 2018-08-21 22:46:58 +0300 (Tue, 21 Aug 2018) $
#$Revision: 210021 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/86/4338629.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_4338629
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         'C38 H34 Al N P2'
_chemical_formula_sum            'C38 H34 Al N P2'
_chemical_formula_weight         593.58
_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                 112.537(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5904(10)
_cell_length_b                   9.7111(5)
_cell_length_c                   18.8411(11)
_cell_measurement_reflns_used    6454
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     3310.7(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0983
_diffrn_reflns_av_sigmaI/netI    0.1064
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10273
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  1.0368
_exptl_absorpt_correction_T_min  0.9207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.282
_refine_ls_extinction_coef       0.039(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   0.977
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0957
_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)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2214
_refine_ls_wR_factor_ref         0.2943
_reflns_number_gt                1795
_reflns_number_total             3008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802030d_si_001.cif
_cod_data_source_block           7813_2a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4338629
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
P1 P 0.11345(6) 0.45187(15) 0.37635(7) 0.0374(6) Uani 1 1 d .
Al1 Al 0.0000 0.5096(2) 0.2500 0.0402(7) Uani 1 2 d S
N1 N 0.0000 0.3098(6) 0.2500 0.0341(14) Uani 1 2 d S
C1 C 0.0562(3) 0.6125(8) 0.2003(4) 0.0637(19) Uani 1 1 d .
H1A H 0.0808 0.5490 0.1791 0.096 Uiso 1 1 calc R
H1B H 0.0922 0.6699 0.2377 0.096 Uiso 1 1 calc R
H1C H 0.0230 0.6690 0.1600 0.096 Uiso 1 1 calc R
C2 C 0.0210(2) 0.2343(6) 0.3192(3) 0.0356(12) Uani 1 1 d .
C3 C -0.0116(3) 0.1094(6) 0.3252(3) 0.0416(13) Uani 1 1 d .
H3 H -0.0495 0.0739 0.2822 0.050 Uiso 1 1 calc R
C4 C 0.0113(3) 0.0372(7) 0.3934(3) 0.0515(15) Uani 1 1 d .
H4 H -0.0102 -0.0475 0.3950 0.062 Uiso 1 1 calc R
C5 C 0.0653(3) 0.0882(7) 0.4593(3) 0.0535(16) Uani 1 1 d .
H5 H 0.0803 0.0391 0.5051 0.064 Uiso 1 1 calc R
C6 C 0.0966(3) 0.2138(7) 0.4555(3) 0.0489(15) Uani 1 1 d .
H6 H 0.1322 0.2504 0.4999 0.059 Uiso 1 1 calc R
C7 C 0.0760(3) 0.2873(6) 0.3869(3) 0.0379(13) Uani 1 1 d .
C8 C 0.1970(2) 0.4131(5) 0.3596(3) 0.0353(12) Uani 1 1 d .
C9 C 0.2181(3) 0.2806(6) 0.3508(3) 0.0391(13) Uani 1 1 d .
H9 H 0.1905 0.2062 0.3563 0.047 Uiso 1 1 calc R
C10 C 0.2798(3) 0.2581(6) 0.3340(3) 0.0456(14) Uani 1 1 d .
H10 H 0.2939 0.1684 0.3287 0.055 Uiso 1 1 calc R
C11 C 0.3208(3) 0.3671(6) 0.3248(3) 0.0434(14) Uani 1 1 d .
H11 H 0.3618 0.3516 0.3126 0.052 Uiso 1 1 calc R
C12 C 0.3001(3) 0.4985(6) 0.3339(3) 0.0496(15) Uani 1 1 d .
H12 H 0.3279 0.5727 0.3287 0.060 Uiso 1 1 calc R
C13 C 0.2383(3) 0.5221(6) 0.3509(3) 0.0488(15) Uani 1 1 d .
H13 H 0.2245 0.6118 0.3564 0.059 Uiso 1 1 calc R
C14 C 0.1452(3) 0.5272(6) 0.4726(3) 0.0411(13) Uani 1 1 d .
C15 C 0.2188(3) 0.5300(6) 0.5224(3) 0.0498(15) Uani 1 1 d .
H15 H 0.2554 0.4957 0.5072 0.060 Uiso 1 1 calc R
C16 C 0.2369(4) 0.5847(7) 0.5952(3) 0.0596(17) Uani 1 1 d .
H16 H 0.2860 0.5860 0.6293 0.071 Uiso 1 1 calc R
C17 C 0.1839(4) 0.6365(7) 0.6176(3) 0.0618(18) Uani 1 1 d .
H17 H 0.1969 0.6720 0.6669 0.074 Uiso 1 1 calc R
C18 C 0.1114(4) 0.6368(8) 0.5681(4) 0.0663(19) Uani 1 1 d .
H18 H 0.0754 0.6739 0.5833 0.080 Uiso 1 1 calc R
C19 C 0.0922(3) 0.5825(7) 0.4963(3) 0.0574(17) Uani 1 1 d .
H19 H 0.0429 0.5826 0.4628 0.069 Uiso 1 1 calc R
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'
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 C8 105.5(2) . .
C7 P1 C14 104.1(2) . .
C8 P1 C14 105.5(2) . .
C7 P1 Al1 92.91(16) . .
C8 P1 Al1 113.14(16) . .
C14 P1 Al1 131.49(19) . .
N1 Al1 C1 120.5(2) . 2
N1 Al1 C1 120.5(2) . .
C1 Al1 C1 119.0(5) 2 .
N1 Al1 P1 77.64(6) . 2
C1 Al1 P1 96.12(18) 2 2
C1 Al1 P1 96.36(18) . 2
N1 Al1 P1 77.64(6) . .
C1 Al1 P1 96.36(18) 2 .
C1 Al1 P1 96.12(18) . .
P1 Al1 P1 155.28(12) 2 .
C2 N1 C2 117.4(6) . 2
C2 N1 Al1 121.3(3) . .
C2 N1 Al1 121.3(3) 2 .
Al1 C1 H1A 109.5 . .
Al1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Al1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 N1 123.1(4) . .
C3 C2 C7 117.2(4) . .
N1 C2 C7 119.7(5) . .
C4 C3 C2 121.4(5) . .
C4 C3 H3 119.3 . .
C2 C3 H3 119.3 . .
C3 C4 C5 121.3(6) . .
C3 C4 H4 119.3 . .
C5 C4 H4 119.3 . .
C6 C5 C4 118.3(5) . .
C6 C5 H5 120.8 . .
C4 C5 H5 120.8 . .
C5 C6 C7 121.6(5) . .
C5 C6 H6 119.2 . .
C7 C6 H6 119.2 . .
C6 C7 C2 120.0(5) . .
C6 C7 P1 124.8(4) . .
C2 C7 P1 115.2(4) . .
C13 C8 C9 119.0(5) . .
C13 C8 P1 118.0(4) . .
C9 C8 P1 122.9(4) . .
C10 C9 C8 120.3(5) . .
C10 C9 H9 119.9 . .
C8 C9 H9 119.9 . .
C11 C10 C9 120.7(5) . .
C11 C10 H10 119.7 . .
C9 C10 H10 119.7 . .
C12 C11 C10 119.1(5) . .
C12 C11 H11 120.4 . .
C10 C11 H11 120.4 . .
C11 C12 C13 120.6(5) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C8 C13 C12 120.4(5) . .
C8 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C19 C14 C15 119.1(5) . .
C19 C14 P1 117.6(4) . .
C15 C14 P1 123.3(4) . .
C14 C15 C16 118.9(6) . .
C14 C15 H15 120.5 . .
C16 C15 H15 120.5 . .
C17 C16 C15 120.9(6) . .
C17 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
C16 C17 C18 120.4(6) . .
C16 C17 H17 119.8 . .
C18 C17 H17 119.8 . .
C17 C18 C19 119.6(6) . .
C17 C18 H18 120.2 . .
C19 C18 H18 120.2 . .
C18 C19 C14 121.0(6) . .
C18 C19 H19 119.5 . .
C14 C19 H19 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C7 1.801(6) .
P1 C8 1.821(5) .
P1 C14 1.829(5) .
P1 Al1 2.6202(13) .
Al1 N1 1.940(7) .
Al1 C1 1.968(6) 2
Al1 C1 1.968(6) .
Al1 P1 2.6202(13) 2
N1 C2 1.413(6) .
N1 C2 1.413(6) 2
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C3 1.395(7) .
C2 C7 1.414(7) .
C3 C4 1.379(8) .
C3 H3 0.9300 .
C4 C5 1.377(8) .
C4 H4 0.9300 .
C5 C6 1.379(8) .
C5 H5 0.9300 .
C6 C7 1.394(7) .
C6 H6 0.9300 .
C8 C13 1.379(7) .
C8 C9 1.381(7) .
C9 C10 1.381(7) .
C9 H9 0.9300 .
C10 C11 1.378(8) .
C10 H10 0.9300 .
C11 C12 1.370(8) .
C11 H11 0.9300 .
C12 C13 1.385(8) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 C19 1.385(8) .
C14 C15 1.387(7) .
C15 C16 1.385(9) .
C15 H15 0.9300 .
C16 C17 1.359(9) .
C16 H16 0.9300 .
C17 C18 1.368(9) .
C17 H17 0.9300 .
C18 C19 1.364(8) .
C18 H18 0.9300 .
C19 H19 0.9300 .
