#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:34:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180268 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/54/7115475.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_7115475
loop_
_publ_author_name
'Adi E. Nako'
'Sarah J. Gates'
'Nicole Schadel'
'Andrew J. P. White'
'Mark R. Crimmin'
_publ_section_title
;
 Yttrium-catalysed dehydrocoupling of alanes with amines
;
_journal_name_full               Chem.Commun.
_journal_page_first              9536
_journal_paper_doi               10.1039/C4cc04484C
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C29 H35 Al F N3'
_chemical_formula_sum            'C29 H35 Al F N3'
_chemical_formula_weight         471.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.11825(9)
_cell_length_b                   19.66971(14)
_cell_length_c                   9.20725(6)
_cell_measurement_reflns_used    13318
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.2859
_cell_measurement_theta_min      2.2443
_cell_volume                     2737.97(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21297
_diffrn_reflns_theta_full        72.44
_diffrn_reflns_theta_max         72.44
_diffrn_reflns_theta_min         4.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0406
_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)+(0.0716P)²+0.6130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                2591
_reflns_number_total             2788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04484c2.cif
_cod_data_source_block           2a
_cod_original_cell_volume        2737.98(3)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7115475
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Al Al 0.35020(3) 0.2500 0.65008(6) 0.03531(17) Uani 1 2 d S
H H 0.4290(16) 0.2500 0.756(3) 0.045(6) Uiso 1 2 d S
C1 C 0.18230(8) 0.31384(7) 0.69741(13) 0.0407(3) Uani 1 1 d .
N1 N 0.26991(7) 0.32167(6) 0.68588(11) 0.0384(3) Uani 1 1 d .
C2 C 0.14179(11) 0.2500 0.69669(19) 0.0410(4) Uani 1 2 d S
H2A H 0.0790 0.2500 0.6956 0.049 Uiso 1 2 calc SR
C3 C 0.12426(10) 0.37550(9) 0.71438(19) 0.0585(4) Uani 1 1 d .
H3A H 0.1392 0.3989 0.8051 0.088 Uiso 1 1 calc R
H3B H 0.0621 0.3614 0.7169 0.088 Uiso 1 1 calc R
H3C H 0.1337 0.4063 0.6322 0.088 Uiso 1 1 calc R
C4 C 0.31060(9) 0.38767(7) 0.69961(15) 0.0430(3) Uani 1 1 d .
C5 C 0.32570(10) 0.42792(8) 0.57617(18) 0.0519(4) Uani 1 1 d .
C6 C 0.37481(12) 0.48725(8) 0.5942(2) 0.0639(4) Uani 1 1 d .
H6A H 0.3855 0.5150 0.5116 0.077 Uiso 1 1 calc R
C7 C 0.40887(12) 0.50760(8) 0.7272(2) 0.0635(4) Uani 1 1 d .
C8 C 0.39089(12) 0.46748(8) 0.8470(2) 0.0584(4) Uani 1 1 d .
H8A H 0.4126 0.4811 0.9393 0.070 Uiso 1 1 calc R
C9 C 0.34203(10) 0.40783(8) 0.83637(17) 0.0479(3) Uani 1 1 d .
C10 C 0.29117(13) 0.40830(10) 0.42879(18) 0.0649(5) Uani 1 1 d .
H10A H 0.2839 0.4492 0.3692 0.097 Uiso 1 1 calc R
H10B H 0.2339 0.3855 0.4395 0.097 Uiso 1 1 calc R
H10C H 0.3332 0.3774 0.3817 0.097 Uiso 1 1 calc R
C11 C 0.46422(18) 0.57130(10) 0.7411(4) 0.0938(7) Uani 1 1 d .
H11A H 0.4406 0.5997 0.8194 0.141 Uiso 1 1 calc R
H11B H 0.4624 0.5966 0.6494 0.141 Uiso 1 1 calc R
H11C H 0.5255 0.5588 0.7633 0.141 Uiso 1 1 calc R
C12 C 0.32290(13) 0.36607(9) 0.96986(17) 0.0603(4) Uani 1 1 d .
H12A H 0.3536 0.3859 1.0535 0.090 Uiso 1 1 calc R
H12B H 0.3436 0.3194 0.9547 0.090 Uiso 1 1 calc R
H12C H 0.2590 0.3657 0.9882 0.090 Uiso 1 1 calc R
N13 N 0.38231(10) 0.2500 0.46034(17) 0.0443(4) Uani 1 2 d SD
H13 H 0.3348(12) 0.2500 0.401(3) 0.073(8) Uiso 1 2 d SD
C14 C 0.46151(11) 0.2500 0.38561(19) 0.0354(4) Uani 1 2 d S
C15 C 0.46347(13) 0.2500 0.2339(2) 0.0422(4) Uani 1 2 d S
H15A H 0.4092 0.2500 0.1819 0.051 Uiso 1 2 calc SR
C16 C 0.54198(16) 0.2500 0.1575(2) 0.0521(5) Uani 1 2 d S
H16A H 0.5421 0.2500 0.0544 0.063 Uiso 1 2 calc SR
C17 C 0.61914(15) 0.2500 0.2335(3) 0.0552(5) Uani 1 2 d S
F17 F 0.69768(11) 0.2500 0.1591(2) 0.0911(6) Uani 1 2 d S
C18 C 0.62161(13) 0.2500 0.3829(3) 0.0560(5) Uani 1 2 d S
H18A H 0.6765 0.2500 0.4331 0.067 Uiso 1 2 calc SR
C19 C 0.54237(12) 0.2500 0.4584(2) 0.0452(4) Uani 1 2 d S
H19A H 0.5431 0.2500 0.5615 0.054 Uiso 1 2 calc SR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 '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
N13 Al N1 109.89(5) . 7_565
N13 Al N1 109.89(5) . .
N1 Al N1 96.52(7) 7_565 .
N1 C1 C2 122.49(12) . .
N1 C1 C3 119.52(13) . .
C2 C1 C3 117.99(12) . .
C1 N1 C4 121.27(11) . .
C1 N1 Al 124.34(10) . .
C4 N1 Al 114.39(8) . .
C1 C2 C1 128.00(16) . 7_565
C9 C4 C5 120.80(14) . .
C9 C4 N1 118.53(12) . .
C5 C4 N1 120.40(13) . .
C6 C5 C4 117.56(16) . .
C6 C5 C10 120.48(15) . .
C4 C5 C10 121.96(15) . .
C7 C6 C5 122.99(16) . .
C8 C7 C6 117.78(15) . .
C8 C7 C11 121.0(2) . .
C6 C7 C11 121.25(19) . .
C7 C8 C9 122.03(16) . .
C8 C9 C4 118.79(14) . .
C8 C9 C12 120.34(15) . .
C4 C9 C12 120.87(13) . .
C14 N13 Al 135.41(13) . .
N13 C14 C19 121.40(16) . .
N13 C14 C15 121.09(16) . .
C19 C14 C15 117.51(16) . .
C16 C15 C14 121.86(19) . .
C17 C16 C15 118.41(19) . .
C16 C17 F17 119.1(2) . .
C16 C17 C18 122.49(19) . .
F17 C17 C18 118.4(2) . .
C17 C18 C19 118.6(2) . .
C18 C19 C14 121.16(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al N13 1.8132(16) .
Al N1 1.8893(11) 7_565
Al N1 1.8893(11) .
C1 N1 1.3377(16) .
C1 C2 1.3971(16) .
C1 C3 1.505(2) .
N1 C4 1.4420(18) .
C2 C1 1.3971(16) 7_565
C4 C9 1.403(2) .
C4 C5 1.404(2) .
C5 C6 1.393(2) .
C5 C10 1.504(2) .
C6 C7 1.388(3) .
C7 C8 1.383(3) .
C7 C11 1.512(3) .
C8 C9 1.390(2) .
C9 C12 1.506(2) .
N13 C14 1.381(2) .
C14 C19 1.394(2) .
C14 C15 1.397(3) .
C15 C16 1.380(3) .
C16 C17 1.360(4) .
C17 F17 1.371(2) .
C17 C18 1.376(4) .
C18 C19 1.385(3) .
