#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:33:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179146 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/07/4310761.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_4310761
loop_
_publ_author_name
'Lan-Chang Liang'
'Mei-Hui Huang'
'Chen-Hsiung Hung'
_publ_section_title
;
 Aluminum Complexes Incorporating Bidentate Amido Phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2166
_journal_page_last               2174
_journal_paper_doi               10.1021/ic035373q
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C34 H39 Al Cl2 N O2 P'
_chemical_formula_weight         622.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.000(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.355(2)
_cell_length_b                   9.997(2)
_cell_length_c                   34.033(7)
_cell_measurement_temperature    150(2)
_cell_volume                     3182.8(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.1660
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            10934
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.5885
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            0.40
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0504P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                2760
_reflns_number_total             6147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035373qsi20031127_125053_2.cif
_cod_data_source_block           '[Me_NP]AlCl2(THF)'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3182.9(12)
_cod_database_code               4310761
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.02071(14) 0.03557(16) 0.15069(5) 0.0254(4) Uani 1 1 d . . .
C1 C 0.3733(5) -0.1727(5) 0.14454(15) 0.0282(13) Uani 1 1 d . . .
C2 C 0.5189(5) -0.1437(6) 0.14466(16) 0.0335(14) Uani 1 1 d . . .
H2 H 0.5520 -0.0652 0.1319 0.040 Uiso 1 1 calc R . .
C3 C 0.6155(6) -0.2264(6) 0.16294(19) 0.0480(18) Uani 1 1 d . . .
H3 H 0.7142 -0.2041 0.1628 0.058 Uiso 1 1 calc R . .
C4 C 0.5708(5) -0.3405(6) 0.18134(17) 0.0400(16) Uani 1 1 d . . .
H4 H 0.6380 -0.3979 0.1938 0.048 Uiso 1 1 calc R . .
C5 C 0.4258(5) -0.3718(6) 0.18171(16) 0.0361(15) Uani 1 1 d . . .
H5 H 0.3945 -0.4527 0.1936 0.043 Uiso 1 1 calc R . .
C6 C 0.3281(5) -0.2874(6) 0.16518(15) 0.0299(14) Uani 1 1 d . . .
H6 H 0.2290 -0.3062 0.1676 0.036 Uiso 1 1 calc R . .
C7 C 0.2246(4) -0.1635(6) 0.07112(15) 0.0240(13) Uani 1 1 d . . .
C8 C 0.2458(5) -0.3032(6) 0.06756(16) 0.0277(13) Uani 1 1 d . . .
H8 H 0.2689 -0.3544 0.0902 0.033 Uiso 1 1 calc R . .
C9 C 0.2335(5) -0.3659(6) 0.03178(17) 0.0309(14) Uani 1 1 d . . .
H9 H 0.2489 -0.4597 0.0301 0.037 Uiso 1 1 calc R . .
C10 C 0.1997(5) -0.2965(7) -0.0011(2) 0.0418(16) Uani 1 1 d . . .
H10 H 0.1926 -0.3408 -0.0257 0.050 Uiso 1 1 calc R . .
C11 C 0.1757(5) -0.1593(7) 0.00160(19) 0.0417(16) Uani 1 1 d . . .
H11 H 0.1510 -0.1097 -0.0212 0.050 Uiso 1 1 calc R . .
C12 C 0.1876(5) -0.0959(6) 0.03720(17) 0.0346(15) Uani 1 1 d . . .
H12 H 0.1699 -0.0024 0.0386 0.042 Uiso 1 1 calc R . .
C13 C 0.3210(5) 0.0829(5) 0.10524(15) 0.0246(13) Uani 1 1 d . . .
C14 C 0.4386(5) 0.0963(6) 0.07994(16) 0.0345(15) Uani 1 1 d . . .
H14 H 0.4747 0.0193 0.0669 0.041 Uiso 1 1 calc R . .
C15 C 0.5034(5) 0.2188(6) 0.07345(17) 0.0396(16) Uani 1 1 d . . .
H15 H 0.5824 0.2264 0.0561 0.048 Uiso 1 1 calc R . .
C16 C 0.4510(5) 0.3290(6) 0.09271(16) 0.0348(15) Uani 1 1 d . . .
H16 H 0.4967 0.4130 0.0893 0.042 Uiso 1 1 calc R . .
C17 C 0.3314(5) 0.3200(5) 0.11729(15) 0.0286(13) Uani 1 1 d . . .
H17 H 0.2966 0.3980 0.1300 0.034 Uiso 1 1 calc R . .
C18 C 0.2620(5) 0.1965(5) 0.12343(14) 0.0213(12) Uani 1 1 d . . .
C19 C 0.0941(5) 0.3106(5) 0.16460(16) 0.0243(13) Uani 1 1 d . . .
C20 C 0.0152(5) 0.4056(6) 0.1443(2) 0.0386(16) Uani 1 1 d . . .
C21 C -0.0256(7) 0.5203(7) 0.1648(3) 0.068(3) Uani 1 1 d . . .
H21 H -0.0784 0.5874 0.1514 0.081 Uiso 1 1 calc R . .
C22 C 0.0076(8) 0.5397(8) 0.2035(3) 0.090(4) Uani 1 1 d . . .
H22 H -0.0261 0.6169 0.2169 0.108 Uiso 1 1 calc R . .
C23 C 0.0909(7) 0.4462(8) 0.2232(2) 0.063(2) Uani 1 1 d . . .
H23 H 0.1171 0.4613 0.2498 0.075 Uiso 1 1 calc R . .
C24 C 0.1362(5) 0.3302(6) 0.20411(18) 0.0365(16) Uani 1 1 d . . .
C25 C -0.0163(6) 0.3885(7) 0.1021(2) 0.062(2) Uani 1 1 d . . .
H25A H 0.0657 0.4187 0.0866 0.093 Uiso 1 1 calc R . .
H25B H -0.1007 0.4416 0.0952 0.093 Uiso 1 1 calc R . .
H25C H -0.0349 0.2939 0.0966 0.093 Uiso 1 1 calc R . .
C26 C 0.2328(6) 0.2330(7) 0.22580(18) 0.0516(19) Uani 1 1 d . . .
H26A H 0.2422 0.2611 0.2533 0.077 Uiso 1 1 calc R . .
H26B H 0.3273 0.2320 0.2134 0.077 Uiso 1 1 calc R . .
H26C H 0.1912 0.1431 0.2248 0.077 Uiso 1 1 calc R . .
C27 C -0.2635(5) 0.1915(6) 0.15569(16) 0.0342(15) Uani 1 1 d . . .
H27A H -0.3113 0.1269 0.1380 0.041 Uiso 1 1 calc R . .
H27B H -0.2307 0.2689 0.1400 0.041 Uiso 1 1 calc R . .
C28 C -0.3645(6) 0.2365(7) 0.18760(19) 0.055(2) Uani 1 1 d . . .
H28A H -0.4146 0.3199 0.1801 0.067 Uiso 1 1 calc R . .
H28B H -0.4361 0.1665 0.1937 0.067 Uiso 1 1 calc R . .
C29 C -0.2663(6) 0.2589(6) 0.22135(17) 0.0435(16) Uani 1 1 d . . .
H29A H -0.3186 0.2549 0.2466 0.052 Uiso 1 1 calc R . .
H29B H -0.2179 0.3467 0.2192 0.052 Uiso 1 1 calc R . .
C30 C -0.1602(5) 0.1459(6) 0.21813(15) 0.0332(14) Uani 1 1 d . . .
H30A H -0.0683 0.1698 0.2307 0.040 Uiso 1 1 calc R . .
H30B H -0.1978 0.0634 0.2305 0.040 Uiso 1 1 calc R . .
C31 C 0.8505(5) 0.6520(6) 0.03705(19) 0.0461(17) Uani 1 1 d . . .
H31A H 0.9149 0.5927 0.0219 0.055 Uiso 1 1 calc R . .
H31B H 0.9057 0.6930 0.0588 0.055 Uiso 1 1 calc R . .
C32 C 0.7895(6) 0.7580(6) 0.0110(2) 0.0522(18) Uani 1 1 d . . .
H32A H 0.7755 0.7250 -0.0161 0.063 Uiso 1 1 calc R . .
H32B H 0.8510 0.8386 0.0105 0.063 Uiso 1 1 calc R . .
C33 C 0.6468(6) 0.7859(7) 0.0314(2) 0.0571(19) Uani 1 1 d . . .
H33A H 0.6585 0.8497 0.0534 0.068 Uiso 1 1 calc R . .
H33B H 0.5755 0.8217 0.0126 0.068 Uiso 1 1 calc R . .
C34 C 0.6046(6) 0.6507(7) 0.0459(2) 0.074(2) Uani 1 1 d . . .
H34A H 0.5499 0.6584 0.0707 0.089 Uiso 1 1 calc R . .
H34B H 0.5441 0.6046 0.0262 0.089 Uiso 1 1 calc R . .
Cl1 Cl -0.10846(13) -0.02361(16) 0.10059(4) 0.0404(4) Uani 1 1 d . . .
Cl2 Cl 0.03280(14) -0.10041(14) 0.20003(4) 0.0386(4) Uani 1 1 d . . .
N1 N 0.1374(4) 0.1868(4) 0.14640(12) 0.0215(10) Uani 1 1 d . . .
O1 O -0.1430(3) 0.1283(3) 0.17564(10) 0.0284(9) Uani 1 1 d . . .
O2 O 0.7329(4) 0.5781(4) 0.05220(13) 0.0551(13) Uani 1 1 d . . .
P1 P 0.23955(13) -0.07521(14) 0.11744(4) 0.0259(4) 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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
N1 Al1 O1 96.09(17) . . ?
N1 Al1 Cl2 122.54(15) . . ?
O1 Al1 Cl2 90.11(12) . . ?
N1 Al1 Cl1 118.92(15) . . ?
O1 Al1 Cl1 91.95(12) . . ?
Cl2 Al1 Cl1 117.85(9) . . ?
N1 Al1 P1 81.37(13) . . ?
O1 Al1 P1 177.42(13) . . ?
Cl2 Al1 P1 91.67(7) . . ?
Cl1 Al1 P1 88.87(7) . . ?
C2 C1 C6 117.5(5) . . ?
C2 C1 P1 123.9(4) . . ?
C6 C1 P1 118.6(4) . . ?
C3 C2 C1 121.3(5) . . ?
C4 C3 C2 120.6(5) . . ?
C3 C4 C5 119.3(5) . . ?
C6 C5 C4 120.6(5) . . ?
C5 C6 C1 120.5(5) . . ?
C12 C7 C8 116.5(5) . . ?
C12 C7 P1 120.5(4) . . ?
C8 C7 P1 123.0(4) . . ?
C9 C8 C7 120.9(5) . . ?
C10 C9 C8 121.1(6) . . ?
C9 C10 C11 119.3(6) . . ?
C12 C11 C10 120.0(6) . . ?
C11 C12 C7 122.2(6) . . ?
C14 C13 C18 120.0(5) . . ?
C14 C13 P1 123.8(4) . . ?
C18 C13 P1 116.2(4) . . ?
C15 C14 C13 121.7(5) . . ?
C16 C15 C14 118.5(5) . . ?
C15 C16 C17 121.3(5) . . ?
C16 C17 C18 120.9(5) . . ?
N1 C18 C13 120.9(4) . . ?
N1 C18 C17 121.6(5) . . ?
C13 C18 C17 117.4(4) . . ?
C20 C19 C24 121.8(5) . . ?
C20 C19 N1 121.5(5) . . ?
C24 C19 N1 116.7(5) . . ?
C19 C20 C21 117.3(7) . . ?
C19 C20 C25 120.8(5) . . ?
C21 C20 C25 121.8(7) . . ?
C22 C21 C20 122.4(8) . . ?
C21 C22 C23 119.8(7) . . ?
C22 C23 C24 120.3(7) . . ?
C23 C24 C19 118.3(6) . . ?
C23 C24 C26 119.1(6) . . ?
C19 C24 C26 122.6(5) . . ?
O1 C27 C28 106.2(4) . . ?
C29 C28 C27 102.3(4) . . ?
C28 C29 C30 103.8(5) . . ?
O1 C30 C29 103.5(4) . . ?
O2 C31 C32 106.8(4) . . ?
C31 C32 C33 101.2(5) . . ?
C34 C33 C32 102.5(5) . . ?
O2 C34 C33 106.8(5) . . ?
C18 N1 C19 114.3(4) . . ?
C18 N1 Al1 125.7(3) . . ?
C19 N1 Al1 119.7(3) . . ?
C27 O1 C30 108.8(4) . . ?
C27 O1 Al1 126.9(3) . . ?
C30 O1 Al1 124.3(3) . . ?
C34 O2 C31 109.5(4) . . ?
C13 P1 C7 105.0(2) . . ?
C13 P1 C1 107.1(2) . . ?
C7 P1 C1 103.4(2) . . ?
C13 P1 Al1 93.41(17) . . ?
C7 P1 Al1 121.86(15) . . ?
C1 P1 Al1 123.16(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 N1 1.870(4) . ?
Al1 O1 1.981(3) . ?
Al1 Cl2 2.163(2) . ?
Al1 Cl1 2.172(2) . ?
Al1 P1 2.5882(19) . ?
C1 C2 1.392(6) . ?
C1 C6 1.410(7) . ?
C1 P1 1.835(5) . ?
C2 C3 1.374(7) . ?
C3 C4 1.367(8) . ?
C4 C5 1.393(7) . ?
C5 C6 1.365(7) . ?
C7 C12 1.382(7) . ?
C7 C8 1.416(7) . ?
C7 P1 1.812(5) . ?
C8 C9 1.375(7) . ?
C9 C10 1.353(8) . ?
C10 C11 1.392(8) . ?
C11 C12 1.372(7) . ?
C13 C14 1.404(6) . ?
C13 C18 1.406(7) . ?
C13 P1 1.803(5) . ?
C14 C15 1.383(7) . ?
C15 C16 1.373(8) . ?
C16 C17 1.400(6) . ?
C17 C18 1.410(7) . ?
C18 N1 1.407(5) . ?
C19 C20 1.387(7) . ?
C19 C24 1.415(7) . ?
C19 N1 1.442(6) . ?
C20 C21 1.396(9) . ?
C20 C25 1.475(8) . ?
C21 C22 1.366(11) . ?
C22 C23 1.390(11) . ?
C23 C24 1.394(8) . ?
C24 C26 1.519(8) . ?
C27 O1 1.460(5) . ?
C27 C28 1.508(7) . ?
C28 C29 1.488(7) . ?
C29 C30 1.507(7) . ?
C30 O1 1.465(6) . ?
C31 O2 1.422(6) . ?
C31 C32 1.494(8) . ?
C32 C33 1.529(7) . ?
C33 C34 1.493(9) . ?
C34 O2 1.420(7) . ?
