#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:26:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179110 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/72/4307207.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_4307207
loop_
_publ_author_name
'Bing Lian'
'Christophe M. Thomas'
'Osvaldo L. Casagrande'
'Christian W. Lehmann'
'Thierry Roisnel'
'Jean-François Carpentier'
_publ_section_title
;
Aluminum and Zinc Complexes Based on an Amino-Bis(pyrazolyl) Ligand:
Synthesis, Structures, and Use in MMA and Lactide Polymerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              328
_journal_page_last               340
_journal_paper_doi               10.1021/ic061749z
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C17 H32 Al N5'
_chemical_formula_weight         333.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.304(5)
_cell_angle_beta                 93.821(5)
_cell_angle_gamma                106.374(5)
_cell_formula_units_Z            2
_cell_length_a                   8.826(5)
_cell_length_b                   10.920(5)
_cell_length_c                   11.763(5)
_cell_measurement_temperature    293(2)
_cell_volume                     986.9(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.849
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23752
_diffrn_reflns_theta_full        35.47
_diffrn_reflns_theta_max         35.47
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.110
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             364
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.025(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   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         7650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0462
_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)+(0.0851P)²+0.3376P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                6561
_reflns_number_total             7650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061749zsi20060914_055238_1.cif
_cod_data_source_block           Complex_2
_cod_database_code               4307207
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.94290(3) 0.78559(3) 0.74199(3) 0.01654(8) Uani 1 1 d . . .
C1 C 0.80159(14) 0.88733(11) 0.83027(10) 0.0244(2) Uani 1 1 d . . .
H1A H 0.6915 0.8265 0.8013 0.037 Uiso 0.50 1 calc PR . .
H1B H 0.8136 0.9686 0.8133 0.037 Uiso 0.50 1 calc PR . .
H1C H 0.8314 0.9161 0.9188 0.037 Uiso 0.50 1 calc PR . .
H1D H 0.8662 0.9809 0.8877 0.037 Uiso 0.50 1 calc PR . .
H1E H 0.7441 0.8389 0.8756 0.037 Uiso 0.50 1 calc PR . .
H1F H 0.7263 0.8914 0.7702 0.037 Uiso 0.50 1 calc PR . .
C2 C 0.86317(14) 0.67468(12) 0.55938(9) 0.02358(19) Uani 1 1 d . . .
H2A H 0.7505 0.6230 0.5436 0.035 Uiso 0.50 1 calc PR . .
H2B H 0.9213 0.6105 0.5279 0.035 Uiso 0.50 1 calc PR . .
H2C H 0.8791 0.7368 0.5180 0.035 Uiso 0.50 1 calc PR . .
H2D H 0.9501 0.6905 0.5161 0.035 Uiso 0.50 1 calc PR . .
H2E H 0.7793 0.7030 0.5318 0.035 Uiso 0.50 1 calc PR . .
H2F H 0.8215 0.5767 0.5417 0.035 Uiso 0.50 1 calc PR . .
C3 C 1.17423(13) 0.90015(12) 0.79352(10) 0.0253(2) Uani 1 1 d . . .
H3A H 1.2015 0.9499 0.8831 0.038 Uiso 0.50 1 calc PR . .
H3B H 1.1956 0.9662 0.7563 0.038 Uiso 0.50 1 calc PR . .
H3C H 1.2378 0.8400 0.7662 0.038 Uiso 0.50 1 calc PR . .
H3D H 1.2217 0.8875 0.7206 0.038 Uiso 0.50 1 calc PR . .
H3E H 1.2277 0.8712 0.8474 0.038 Uiso 0.50 1 calc PR . .
H3F H 1.1855 0.9974 0.8375 0.038 Uiso 0.50 1 calc PR . .
N1 N 0.92902(9) 0.63389(8) 0.80535(7) 0.01453(14) Uani 1 1 d . . .
H1 H 0.840(3) 0.566(2) 0.766(2) 0.050 Uiso 1 1 d . . .
C11 C 1.05598(11) 0.56837(9) 0.76779(9) 0.01725(16) Uani 1 1 d . . .
H11A H 1.1578 0.6302 0.8240 0.021 Uiso 1 1 calc R . .
H11B H 1.0681 0.5594 0.6839 0.021 Uiso 1 1 calc R . .
C12 C 1.01853(11) 0.42459(10) 0.77001(9) 0.01902(17) Uani 1 1 d . . .
H12A H 1.1144 0.3976 0.7639 0.023 Uiso 1 1 calc R . .
H12B H 0.9889 0.4299 0.8493 0.023 Uiso 1 1 calc R . .
N13 N 0.88812(10) 0.31760(8) 0.66774(8) 0.01722(15) Uani 1 1 d . . .
N14 N 0.77471(10) 0.35438(9) 0.61667(8) 0.01950(15) Uani 1 1 d . . .
C15 C 0.53193(14) 0.23276(14) 0.45090(12) 0.0317(2) Uani 1 1 d . . .
H15A H 0.5313 0.3270 0.4752 0.048 Uiso 0.50 1 calc PR . .
H15B H 0.4343 0.1768 0.4630 0.048 Uiso 0.50 1 calc PR . .
H15C H 0.5395 0.1938 0.3642 0.048 Uiso 0.50 1 calc PR . .
H15D H 0.4721 0.1381 0.3930 0.048 Uiso 0.50 1 calc PR . .
H15E H 0.5691 0.2883 0.4053 0.048 Uiso 0.50 1 calc PR . .
H15F H 0.4639 0.2713 0.5041 0.048 Uiso 0.50 1 calc PR . .
C16 C 0.67312(12) 0.23375(11) 0.52922(9) 0.02176(18) Uani 1 1 d . . .
C17 C 0.72022(14) 0.11947(11) 0.52532(10) 0.0245(2) Uani 1 1 d . . .
H17 H 0.6687 0.0251 0.4730 0.029 Uiso 1 1 calc R . .
C18 C 0.85940(13) 0.17716(10) 0.61569(9) 0.02063(18) Uani 1 1 d . . .
C19 C 0.96907(17) 0.11266(12) 0.65544(12) 0.0302(2) Uani 1 1 d . . .
H19A H 1.0552 0.1846 0.7216 0.045 Uiso 0.50 1 calc PR . .
H19B H 1.0128 0.0658 0.5855 0.045 Uiso 0.50 1 calc PR . .
H19C H 0.9098 0.0460 0.6848 0.045 Uiso 0.50 1 calc PR . .
H19D H 0.9300 0.0130 0.6063 0.045 Uiso 0.50 1 calc PR . .
H19E H 0.9724 0.1319 0.7424 0.045 Uiso 0.50 1 calc PR . .
H19F H 1.0754 0.1516 0.6432 0.045 Uiso 0.50 1 calc PR . .
C21 C 0.93090(11) 0.68190(10) 0.94238(8) 0.01619(15) Uani 1 1 d . . .
H21A H 0.9921 0.7813 0.9848 0.019 Uiso 1 1 calc R . .
H21B H 0.9845 0.6322 0.9748 0.019 Uiso 1 1 calc R . .
C22 C 0.76192(11) 0.65696(10) 0.97090(8) 0.01731(16) Uani 1 1 d . . .
H22A H 0.7692 0.6933 1.0609 0.021 Uiso 1 1 calc R . .
H22B H 0.7090 0.7080 0.9398 0.021 Uiso 1 1 calc R . .
N23 N 0.66546(9) 0.50902(9) 0.91437(7) 0.01740(15) Uani 1 1 d . . .
N24 N 0.70509(10) 0.41985(9) 0.95734(8) 0.02049(16) Uani 1 1 d . . .
C25 C 0.59838(15) 0.16695(13) 0.90643(16) 0.0363(3) Uani 1 1 d . . .
H25A H 0.6868 0.1928 0.9725 0.054 Uiso 0.50 1 calc PR . .
H25B H 0.6109 0.0986 0.8304 0.054 Uiso 0.50 1 calc PR . .
H25C H 0.4992 0.1278 0.9287 0.054 Uiso 0.50 1 calc PR . .
H25D H 0.5111 0.0867 0.8485 0.054 Uiso 0.50 1 calc PR . .
H25E H 0.5871 0.1808 0.9906 0.054 Uiso 0.50 1 calc PR . .
H25F H 0.6987 0.1516 0.8924 0.054 Uiso 0.50 1 calc PR . .
C26 C 0.59563(12) 0.29400(11) 0.88736(10) 0.02226(18) Uani 1 1 d . . .
C27 C 0.48620(12) 0.30251(11) 0.80001(10) 0.02287(19) Uani 1 1 d . . .
H27 H 0.3996 0.2294 0.7414 0.027 Uiso 1 1 calc R . .
C28 C 0.53439(11) 0.44221(11) 0.81949(9) 0.01957(17) Uani 1 1 d . . .
C29 C 0.46908(13) 0.51555(14) 0.75443(11) 0.0279(2) Uani 1 1 d . . .
H29A H 0.5315 0.6136 0.7917 0.042 Uiso 0.50 1 calc PR . .
H29B H 0.3590 0.5041 0.7624 0.042 Uiso 0.50 1 calc PR . .
H29C H 0.4748 0.4761 0.6674 0.042 Uiso 0.50 1 calc PR . .
H29D H 0.3787 0.4489 0.6892 0.042 Uiso 0.50 1 calc PR . .
H29E H 0.5512 0.5584 0.7186 0.042 Uiso 0.50 1 calc PR . .
H29F H 0.4353 0.5865 0.8136 0.042 Uiso 0.50 1 calc PR . .
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'
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
C2 Al1 C3 115.53(5) . . ?
C2 Al1 C1 114.82(6) . . ?
C3 Al1 C1 113.47(6) . . ?
C2 Al1 N1 102.45(5) . . ?
C3 Al1 N1 103.52(5) . . ?
C1 Al1 N1 105.02(5) . . ?
C21 N1 C11 111.69(7) . . ?
C21 N1 Al1 113.97(6) . . ?
C11 N1 Al1 110.80(6) . . ?
N1 C11 C12 113.36(8) . . ?
N13 C12 C11 112.11(8) . . ?
C18 N13 N14 112.48(8) . . ?
C18 N13 C12 127.36(9) . . ?
N14 N13 C12 120.13(8) . . ?
C16 N14 N13 104.93(9) . . ?
N14 C16 C17 110.98(10) . . ?
N14 C16 C15 120.38(10) . . ?
C17 C16 C15 128.63(10) . . ?
C18 C17 C16 105.55(9) . . ?
N13 C18 C17 106.05(9) . . ?
N13 C18 C19 122.02(10) . . ?
C17 C18 C19 131.92(10) . . ?
N1 C21 C22 112.11(7) . . ?
N23 C22 C21 112.09(8) . . ?
C28 N23 N24 112.50(9) . . ?
C28 N23 C22 128.15(9) . . ?
N24 N23 C22 119.35(8) . . ?
C26 N24 N23 104.77(9) . . ?
N24 C26 C27 111.03(10) . . ?
N24 C26 C25 121.05(11) . . ?
C27 C26 C25 127.92(10) . . ?
C28 C27 C26 105.77(9) . . ?
N23 C28 C27 105.93(9) . . ?
N23 C28 C29 122.98(10) . . ?
C27 C28 C29 131.07(10) . . ?
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 C2 1.9797(13) . ?
Al1 C3 1.9800(15) . ?
Al1 C1 1.9865(12) . ?
Al1 N1 2.0370(11) . ?
N1 C21 1.4911(13) . ?
N1 C11 1.4970(13) . ?
C11 C12 1.5214(15) . ?
C12 N13 1.4586(13) . ?
N13 C18 1.3559(14) . ?
N13 N14 1.3616(13) . ?
N14 C16 1.3342(13) . ?
C15 C16 1.4945(17) . ?
C16 C17 1.4085(16) . ?
C17 C18 1.3846(16) . ?
C18 C19 1.4919(16) . ?
C21 C22 1.5225(15) . ?
C22 N23 1.4528(14) . ?
N23 C28 1.3602(13) . ?
N23 N24 1.3667(13) . ?
N24 C26 1.3365(14) . ?
C25 C26 1.4934(18) . ?
C26 C27 1.4100(16) . ?
C27 C28 1.3844(17) . ?
C28 C29 1.4920(16) . ?
