#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:26:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179110 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/72/4307210.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_4307210
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            'C18 H33 N5 Zn'
_chemical_formula_weight         384.86
_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                99.522(5)
_cell_angle_beta                 104.599(5)
_cell_angle_gamma                97.946(5)
_cell_formula_units_Z            2
_cell_length_a                   8.145(5)
_cell_length_b                   8.494(5)
_cell_length_c                   15.292(5)
_cell_measurement_temperature    293(2)
_cell_volume                     991.6(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7970
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         5.16
_exptl_absorpt_coefficient_mu    1.248
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             412
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0501P)²+1.7429P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1453
_reflns_number_gt                3739
_reflns_number_total             4474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061749zsi20060914_055238_4.cif
_cod_data_source_block           complex_9
_cod_database_code               4307210
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
Zn1 Zn 0.22700(6) 0.25992(5) 0.75960(3) 0.03177(15) Uani 1 1 d . . .
N1 N 0.2781(4) 0.4358(4) 0.6733(2) 0.0350(7) Uani 1 1 d . . .
N2 N 0.3065(4) 0.6022(4) 0.6944(2) 0.0314(6) Uani 1 1 d . . .
N3 N 0.2062(4) 0.4761(4) 0.8620(2) 0.0306(6) Uani 1 1 d . . .
H3 H 0.109(7) 0.510(6) 0.853(3) 0.050 Uiso 1 1 d . . .
N4 N 0.1281(4) 0.2461(4) 1.0411(2) 0.0311(6) Uani 1 1 d . . .
C5 C 0.2088(5) 0.1211(4) 1.0585(3) 0.0316(7) Uani 1 1 d . . .
C1 C -0.0049(5) 0.1209(5) 0.6920(3) 0.0382(8) Uani 1 1 d . . .
H1A H 0.0136 0.0217 0.6573 0.046 Uiso 1 1 calc R . .
H1B H -0.0604 0.0905 0.7375 0.046 Uiso 1 1 calc R . .
C2 C -0.1288(6) 0.1941(6) 0.6261(3) 0.0496(10) Uani 1 1 d . . .
H2A H -0.2347 0.1169 0.5982 0.074 Uiso 0.50 1 calc PR . .
H2B H -0.0782 0.2212 0.5790 0.074 Uiso 0.50 1 calc PR . .
H2C H -0.1521 0.2906 0.6595 0.074 Uiso 0.50 1 calc PR . .
H2D H -0.0753 0.3022 0.6262 0.074 Uiso 0.50 1 calc PR . .
H2E H -0.2318 0.1980 0.6454 0.074 Uiso 0.50 1 calc PR . .
H2F H -0.1579 0.1285 0.5649 0.074 Uiso 0.50 1 calc PR . .
C3 C 0.4602(5) 0.2158(4) 0.8224(3) 0.0346(8) Uani 1 1 d . . .
H3A H 0.4949 0.2739 0.8864 0.042 Uiso 1 1 calc R . .
H3B H 0.4490 0.1006 0.8224 0.042 Uiso 1 1 calc R . .
C4 C 0.6027(5) 0.2643(5) 0.7785(3) 0.0458(10) Uani 1 1 d . . .
H4A H 0.7088 0.2393 0.8124 0.069 Uiso 0.50 1 calc PR . .
H4B H 0.6177 0.3788 0.7797 0.069 Uiso 0.50 1 calc PR . .
H4C H 0.5716 0.2053 0.7157 0.069 Uiso 0.50 1 calc PR . .
H4D H 0.5565 0.3097 0.7261 0.069 Uiso 0.50 1 calc PR . .
H4E H 0.6477 0.1701 0.7588 0.069 Uiso 0.50 1 calc PR . .
H4F H 0.6938 0.3436 0.8229 0.069 Uiso 0.50 1 calc PR . .
C11 C 0.2694(7) 0.2236(5) 0.5408(3) 0.0480(10) Uani 1 1 d . . .
H11A H 0.2497 0.1543 0.5822 0.072 Uiso 0.50 1 calc PR . .
H11B H 0.3732 0.2082 0.5243 0.072 Uiso 0.50 1 calc PR . .
H11C H 0.1734 0.1970 0.4860 0.072 Uiso 0.50 1 calc PR . .
H11D H 0.2811 0.2187 0.4795 0.072 Uiso 0.50 1 calc PR . .
H11E H 0.1577 0.1648 0.5374 0.072 Uiso 0.50 1 calc PR . .
H11F H 0.3575 0.1760 0.5757 0.072 Uiso 0.50 1 calc PR . .
C12 C 0.2879(5) 0.3974(5) 0.5872(3) 0.0368(8) Uani 1 1 d . . .
C13 C 0.3179(5) 0.5359(5) 0.5519(3) 0.0385(8) Uani 1 1 d . . .
H13 H 0.3284 0.5400 0.4932 0.046 Uiso 1 1 calc R . .
C14 C 0.3290(5) 0.6658(4) 0.6219(3) 0.0351(8) Uani 1 1 d . . .
C15 C 0.3624(7) 0.8445(5) 0.6258(3) 0.0463(10) Uani 1 1 d . . .
H15A H 0.3622 0.9018 0.6854 0.069 Uiso 0.50 1 calc PR . .
H15B H 0.2738 0.8706 0.5788 0.069 Uiso 0.50 1 calc PR . .
H15C H 0.4728 0.8762 0.6157 0.069 Uiso 0.50 1 calc PR . .
H15D H 0.3770 0.8639 0.5679 0.069 Uiso 0.50 1 calc PR . .
H15E H 0.4654 0.8951 0.6744 0.069 Uiso 0.50 1 calc PR . .
H15F H 0.2664 0.8895 0.6376 0.069 Uiso 0.50 1 calc PR . .
C16 C 0.2960(5) 0.6931(4) 0.7824(2) 0.0337(8) Uani 1 1 d . . .
H16A H 0.1791 0.7122 0.7749 0.040 Uiso 1 1 calc R . .
H16B H 0.3721 0.7981 0.7974 0.040 Uiso 1 1 calc R . .
C17 C 0.3437(5) 0.6089(4) 0.8630(2) 0.0323(7) Uani 1 1 d . . .
H17A H 0.4473 0.5655 0.8615 0.039 Uiso 1 1 calc R . .
H17B H 0.3698 0.6885 0.9204 0.039 Uiso 1 1 calc R . .
C21 C 0.2340(5) 0.4340(4) 0.9533(2) 0.0312(7) Uani 1 1 d . . .
H21A H 0.2428 0.5305 0.9994 0.037 Uiso 1 1 calc R . .
H21B H 0.3420 0.3951 0.9689 0.037 Uiso 1 1 calc R . .
C22 C 0.0872(5) 0.3038(4) 0.9552(2) 0.0335(8) Uani 1 1 d . . .
H22A H -0.0177 0.3480 0.9488 0.040 Uiso 1 1 calc R . .
H22B H 0.0671 0.2134 0.9035 0.040 Uiso 1 1 calc R . .
C23 C 0.2490(5) 0.0066(5) 0.9852(3) 0.0390(8) Uani 1 1 d . . .
H23A H 0.2102 0.0374 0.9269 0.059 Uiso 0.50 1 calc PR . .
H23B H 0.1911 -0.1018 0.9813 0.059 Uiso 0.50 1 calc PR . .
H23C H 0.3714 0.0104 1.0001 0.059 Uiso 0.50 1 calc PR . .
H23D H 0.3049 -0.0734 1.0120 0.059 Uiso 0.50 1 calc PR . .
H23E H 0.3240 0.0658 0.9575 0.059 Uiso 0.50 1 calc PR . .
H23F H 0.1438 -0.0464 0.9388 0.059 Uiso 0.50 1 calc PR . .
C24 C 0.2405(5) 0.1270(4) 1.1517(3) 0.0354(8) Uani 1 1 d . . .
H24 H 0.2927 0.0558 1.1847 0.042 Uiso 1 1 calc R . .
N25 N 0.1093(4) 0.3376(4) 1.1195(2) 0.0315(6) Uani 1 1 d . . .
C26 C 0.1779(5) 0.2631(4) 1.1871(3) 0.0337(8) Uani 1 1 d . . .
C27 C 0.1872(6) 0.3301(5) 1.2856(3) 0.0412(9) Uani 1 1 d . . .
H27A H 0.2394 0.2618 1.3242 0.062 Uiso 0.50 1 calc PR . .
H27B H 0.0727 0.3336 1.2909 0.062 Uiso 0.50 1 calc PR . .
H27C H 0.2553 0.4380 1.3047 0.062 Uiso 0.50 1 calc PR . .
H27D H 0.1389 0.4271 1.2890 0.062 Uiso 0.50 1 calc PR . .
H27E H 0.3056 0.3553 1.3223 0.062 Uiso 0.50 1 calc PR . .
H27F H 0.1230 0.2509 1.3085 0.062 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'
Zn Zn 0.2839 1.4301 '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
C1 Zn1 C3 134.78(16) . . ?
C1 Zn1 N1 106.35(15) . . ?
C3 Zn1 N1 105.53(15) . . ?
C1 Zn1 N3 111.90(14) . . ?
C3 Zn1 N3 101.37(13) . . ?
N1 Zn1 N3 86.23(12) . . ?
C12 N1 N2 105.1(3) . . ?
C12 N1 Zn1 125.4(3) . . ?
N2 N1 Zn1 129.4(2) . . ?
C14 N2 N1 111.4(3) . . ?
C14 N2 C16 126.2(3) . . ?
N1 N2 C16 122.2(3) . . ?
C21 N3 C17 110.6(3) . . ?
C21 N3 Zn1 108.7(2) . . ?
C17 N3 Zn1 105.9(2) . . ?
C5 N4 N25 112.5(3) . . ?
C5 N4 C22 127.4(3) . . ?
N25 N4 C22 119.3(3) . . ?
N4 C5 C24 106.4(3) . . ?
N4 C5 C23 122.9(3) . . ?
C24 C5 C23 130.7(3) . . ?
C2 C1 Zn1 117.0(3) . . ?
C4 C3 Zn1 114.8(3) . . ?
N1 C12 C13 111.1(3) . . ?
N1 C12 C11 120.8(4) . . ?
C13 C12 C11 128.1(4) . . ?
C14 C13 C12 106.0(3) . . ?
N2 C14 C13 106.3(3) . . ?
N2 C14 C15 122.7(3) . . ?
C13 C14 C15 130.9(4) . . ?
N2 C16 C17 114.4(3) . . ?
N3 C17 C16 113.1(3) . . ?
N3 C21 C22 111.4(3) . . ?
N4 C22 C21 110.9(3) . . ?
C5 C24 C26 105.9(3) . . ?
C26 N25 N4 104.3(3) . . ?
N25 C26 C24 110.9(3) . . ?
N25 C26 C27 120.8(3) . . ?
C24 C26 C27 128.3(3) . . ?
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
Zn1 C1 2.006(4) . ?
Zn1 C3 2.017(4) . ?
Zn1 N1 2.214(3) . ?
Zn1 N3 2.263(3) . ?
N1 C12 1.328(5) . ?
N1 N2 1.370(4) . ?
N2 C14 1.352(5) . ?
N2 C16 1.466(4) . ?
N3 C21 1.469(5) . ?
N3 C17 1.471(5) . ?
N4 C5 1.352(4) . ?
N4 N25 1.371(4) . ?
N4 C22 1.454(5) . ?
C5 C24 1.374(5) . ?
C5 C23 1.491(5) . ?
C1 C2 1.513(6) . ?
C3 C4 1.524(6) . ?
C11 C12 1.498(5) . ?
C12 C13 1.389(6) . ?
C13 C14 1.380(5) . ?
C14 C15 1.493(5) . ?
C16 C17 1.520(5) . ?
C21 C22 1.522(5) . ?
C24 C26 1.408(5) . ?
N25 C26 1.344(5) . ?
C26 C27 1.498(5) . ?
