#------------------------------------------------------------------------------
#$Date: 2018-09-01 16:57:16 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210304 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/89/4318947.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_4318947
loop_
_publ_author_name
'Yu, Ru-Ching'
'Hung, Chen-Hsiung'
'Huang, Jui-Hsien'
'Lee, Horng-Yi'
'Chen, Jwu-Ting'
_publ_section_title
;
 Four- and Five-Coordinate Aluminum Ketiminate Complexes:
 Synthesis, Characterization, and Ring-Opening Polymerization
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   24
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6450
_journal_page_last               6455
_journal_paper_doi               10.1021/ic025785j
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C34 H48 Al F N2 O2'
_chemical_formula_weight         562.72
_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                 110.0220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.1082(17)
_cell_length_b                   11.4039(8)
_cell_length_c                   12.8490(9)
_cell_measurement_temperature    293(2)
_cell_volume                     3319.0(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10345
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.781
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.781
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0373
_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)+(0.0516P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                1861
_reflns_number_total             3796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025785j_s6.cif
_cod_data_source_block           hjh039m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318947
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 1.0000 0.35446(6) 0.7500 0.0493(2) Uani 1 2 d S . .
O1 O 0.96741(4) 0.34018(10) 0.85655(9) 0.0646(3) Uani 1 1 d . . .
N1 N 0.92507(5) 0.28668(10) 0.64600(10) 0.0473(3) Uani 1 1 d . . .
F1 F 1.0000 0.50156(11) 0.7500 0.0727(4) Uani 1 2 d S . .
C1 C 0.98810(7) 0.32188(14) 0.96166(14) 0.0562(4) Uani 1 1 d . . .
C2 C 0.94480(8) 0.33863(19) 1.02086(16) 0.0862(6) Uani 1 1 d . . .
H2A H 0.9277 0.4154 1.0051 0.129 Uiso 1 1 calc R . .
H2B H 0.9648 0.3306 1.0992 0.129 Uiso 1 1 calc R . .
H2C H 0.9142 0.2806 0.9962 0.129 Uiso 1 1 calc R . .
C3 C 0.91358(7) 0.26796(13) 0.53855(14) 0.0544(4) Uani 1 1 d . . .
C4 C 0.85346(7) 0.22466(17) 0.46518(14) 0.0778(6) Uani 1 1 d . . .
H4A H 0.8239 0.2810 0.4653 0.117 Uiso 1 1 calc R . .
H4B H 0.8450 0.1510 0.4928 0.117 Uiso 1 1 calc R . .
H4C H 0.8534 0.2146 0.3909 0.117 Uiso 1 1 calc R . .
C5 C 0.95524(7) 0.28768(14) 0.48574(14) 0.0601(4) Uani 1 1 d . . .
H5 H 0.9431 0.2765 0.4095 0.072 Uiso 1 1 calc R . .
C6 C 0.87647(7) 0.26514(14) 0.68672(13) 0.0522(4) Uani 1 1 d . . .
C7 C 0.87122(8) 0.15602(15) 0.73198(14) 0.0647(5) Uani 1 1 d . . .
C8 C 0.82717(9) 0.14192(19) 0.77738(17) 0.0851(6) Uani 1 1 d . . .
H8 H 0.8231 0.0701 0.8083 0.102 Uiso 1 1 calc R . .
C9 C 0.78939(9) 0.2319(2) 0.77762(18) 0.0921(7) Uani 1 1 d . . .
H9 H 0.7604 0.2209 0.8094 0.111 Uiso 1 1 calc R . .
C10 C 0.79431(8) 0.33767(19) 0.73120(16) 0.0786(6) Uani 1 1 d . . .
H10 H 0.7682 0.3977 0.7310 0.094 Uiso 1 1 calc R . .
C11 C 0.83759(7) 0.35722(15) 0.68432(14) 0.0593(4) Uani 1 1 d . . .
C13 C 0.94926(10) 0.01964(18) 0.85321(19) 0.1071(8) Uani 1 1 d . . .
H12A H 0.9707 0.0864 0.8923 0.161 Uiso 1 1 calc R . .
H12B H 0.9765 -0.0411 0.8515 0.161 Uiso 1 1 calc R . .
H12C H 0.9234 -0.0088 0.8902 0.161 Uiso 1 1 calc R . .
C14 C 0.87980(12) -0.05258(19) 0.6713(2) 0.1245(9) Uani 1 1 d . . .
H13A H 0.8576 -0.0306 0.5965 0.187 Uiso 1 1 calc R . .
H13B H 0.8535 -0.0820 0.7067 0.187 Uiso 1 1 calc R . .
H13C H 0.9078 -0.1124 0.6710 0.187 Uiso 1 1 calc R . .
C12 C 0.91281(9) 0.05522(16) 0.73487(16) 0.0802(6) Uani 1 1 d . . .
H14A H 0.9403 0.0817 0.6985 0.096 Uiso 1 1 calc R . .
C15 C 0.84201(8) 0.47596(15) 0.63547(16) 0.0686(5) Uani 1 1 d . . .
H15A H 0.8735 0.4715 0.6035 0.082 Uiso 1 1 calc R . .
C16 C 0.78451(9) 0.50910(19) 0.54153(18) 0.1011(7) Uani 1 1 d . . .
H16A H 0.7750 0.4494 0.4855 0.152 Uiso 1 1 calc R . .
H16B H 0.7897 0.5827 0.5098 0.152 Uiso 1 1 calc R . .
H16C H 0.7530 0.5159 0.5708 0.152 Uiso 1 1 calc R . .
C17 C 0.85895(9) 0.57029(18) 0.72399(19) 0.0976(7) Uani 1 1 d . . .
H17A H 0.8953 0.5491 0.7808 0.146 Uiso 1 1 calc R . .
H17B H 0.8284 0.5779 0.7557 0.146 Uiso 1 1 calc R . .
H17C H 0.8639 0.6436 0.6915 0.146 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
Al Al 0.0645 0.0514 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
F1 Al1 O1 95.18(4) . . ?
F1 Al1 O1 95.18(4) . 2_756 ?
O1 Al1 O1 169.64(8) . 2_756 ?
F1 Al1 N1 112.76(4) . . ?
O1 Al1 N1 86.77(5) . . ?
O1 Al1 N1 89.22(5) 2_756 . ?
F1 Al1 N1 112.76(4) . 2_756 ?
O1 Al1 N1 89.22(5) . 2_756 ?
O1 Al1 N1 86.77(5) 2_756 2_756 ?
N1 Al1 N1 134.49(7) . 2_756 ?
C1 O1 Al1 134.29(10) . . ?
C3 N1 C6 116.00(12) . . ?
C3 N1 Al1 125.17(10) . . ?
C6 N1 Al1 118.59(9) . . ?
O1 C1 C5 122.12(15) . 2_756 ?
O1 C1 C2 115.14(15) . . ?
C5 C1 C2 122.73(16) 2_756 . ?
N1 C3 C5 123.03(15) . . ?
N1 C3 C4 120.88(14) . . ?
C5 C3 C4 116.09(15) . . ?
C1 C5 C3 124.58(16) 2_756 . ?
C7 C6 C11 121.43(15) . . ?
C7 C6 N1 119.84(14) . . ?
C11 C6 N1 118.66(14) . . ?
C8 C7 C6 118.06(17) . . ?
C8 C7 C12 119.81(17) . . ?
C6 C7 C12 122.11(15) . . ?
C9 C8 C7 121.28(19) . . ?
C10 C9 C8 120.08(19) . . ?
C9 C10 C11 121.34(19) . . ?
C10 C11 C6 117.79(16) . . ?
C10 C11 C15 119.60(16) . . ?
C6 C11 C15 122.60(14) . . ?
C7 C12 C13 112.06(17) . . ?
C7 C12 C14 112.03(17) . . ?
C13 C12 C14 109.45(17) . . ?
C11 C15 C17 111.30(16) . . ?
C11 C15 C16 111.86(15) . . ?
C17 C15 C16 110.64(16) . . ?
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 F1 1.6775(14) . ?
Al1 O1 1.8041(10) . ?
Al1 O1 1.8041(10) 2_756 ?
Al1 N1 1.9984(12) . ?
Al1 N1 1.9984(12) 2_756 ?
O1 C1 1.2865(18) . ?
N1 C3 1.3290(18) . ?
N1 C6 1.4583(17) . ?
C1 C5 1.357(2) 2_756 ?
C1 C2 1.500(2) . ?
C3 C5 1.410(2) . ?
C3 C4 1.516(2) . ?
C5 C1 1.357(2) 2_756 ?
C6 C7 1.397(2) . ?
C6 C11 1.401(2) . ?
C7 C8 1.385(2) . ?
C7 C12 1.517(2) . ?
C8 C9 1.373(3) . ?
C9 C10 1.369(3) . ?
C10 C11 1.390(2) . ?
C11 C15 1.512(2) . ?
C13 C12 1.528(3) . ?
C14 C12 1.538(3) . ?
C15 C17 1.516(2) . ?
C15 C16 1.541(2) . ?
