#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:26:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179110 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/72/4307214.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_4307214
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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H32 Cl1 N5 Zn1'
_chemical_formula_sum            'C22 H32 Cl N5 Zn'
_chemical_formula_weight         467.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-11-03T17:22:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.436(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.675(2)
_cell_length_b                   21.637(5)
_cell_length_c                   12.645(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.62
_cell_measurement_wavelength     0.71073
_cell_volume                     2276.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare al, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28850
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0380P)²+1.4631P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                4722
_reflns_number_total             5221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061749zsi20060914_055238_8.cif
_cod_data_source_block           bl8
_cod_original_cell_volume        2276.5(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4307214
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.0664(2) 0.17524(8) 0.26647(15) 0.0252(4) Uani 1 1 d . . .
H1A H -0.017(3) 0.1958(13) 0.257(2) 0.05 Uiso 1 1 d . . .
H1B H 0.098(3) 0.1622(12) 0.338(2) 0.05 Uiso 1 1 d . . .
C2 C 0.2076(2) 0.20287(7) 0.23696(14) 0.0214(3) Uani 1 1 d . . .
C3 C 0.1862(2) 0.24262(7) 0.14730(14) 0.0223(3) Uani 1 1 d . . .
H3 H 0.0807 0.2561 0.1097 0.027 Uiso 1 1 calc R . .
C4 C 0.3147(2) 0.26334(8) 0.11089(14) 0.0243(3) Uani 1 1 d . . .
H4 H 0.2943 0.29 0.0488 0.029 Uiso 1 1 calc R . .
C5 C 0.3668(2) 0.18698(8) 0.29149(14) 0.0260(4) Uani 1 1 d . . .
H5 H 0.3878 0.1614 0.355 0.031 Uiso 1 1 calc R . .
C6 C 0.4960(2) 0.20778(8) 0.25495(15) 0.0280(4) Uani 1 1 d . . .
H6 H 0.6021 0.1955 0.2937 0.034 Uiso 1 1 calc R . .
C7 C 0.4723(2) 0.24582(8) 0.16340(14) 0.0252(4) Uani 1 1 d . . .
C8 C 0.6116(2) 0.26669(10) 0.12183(18) 0.0370(4) Uani 1 1 d . . .
H8A H 0.5712 0.2931 0.0569 0.055 Uiso 0.5 1 calc PR . .
H8B H 0.6651 0.2305 0.1018 0.055 Uiso 0.5 1 calc PR . .
H8C H 0.6884 0.29 0.1799 0.055 Uiso 0.5 1 calc PR . .
H8D H 0.7119 0.2493 0.1688 0.055 Uiso 0.5 1 calc PR . .
H8E H 0.6181 0.3119 0.1239 0.055 Uiso 0.5 1 calc PR . .
H8F H 0.5947 0.2524 0.0459 0.055 Uiso 0.5 1 calc PR . .
C11 C -0.1855(2) 0.17842(8) -0.07617(15) 0.0262(4) Uani 1 1 d . . .
H11A H -0.2284 0.1606 -0.019 0.039 Uiso 0.5 1 calc PR . .
H11B H -0.2536 0.1662 -0.1491 0.039 Uiso 0.5 1 calc PR . .
H11C H -0.1842 0.2236 -0.0702 0.039 Uiso 0.5 1 calc PR . .
H11D H -0.2158 0.2063 -0.1398 0.039 Uiso 0.5 1 calc PR . .
H11E H -0.1905 0.2007 -0.0098 0.039 Uiso 0.5 1 calc PR . .
H11F H -0.2599 0.1433 -0.0887 0.039 Uiso 0.5 1 calc PR . .
C12 C -0.01761(19) 0.15529(7) -0.06125(13) 0.0175(3) Uani 1 1 d . . .
C13 C 0.08940(19) 0.16838(7) -0.12305(13) 0.0198(3) Uani 1 1 d . . .
H13 H 0.0702 0.1947 -0.1856 0.024 Uiso 1 1 calc R . .
C14 C 0.22770(19) 0.13567(7) -0.07539(13) 0.0187(3) Uani 1 1 d . . .
C15 C 0.3835(2) 0.13222(10) -0.10424(16) 0.0304(4) Uani 1 1 d . . .
H15A H 0.4572 0.1043 -0.0528 0.046 Uiso 0.5 1 calc PR . .
H15B H 0.4314 0.1735 -0.0992 0.046 Uiso 0.5 1 calc PR . .
H15C H 0.3639 0.1165 -0.1796 0.046 Uiso 0.5 1 calc PR . .
H15D H 0.3778 0.1586 -0.1682 0.046 Uiso 0.5 1 calc PR . .
H15E H 0.4036 0.0894 -0.1219 0.046 Uiso 0.5 1 calc PR . .
H15F H 0.4711 0.1464 -0.0415 0.046 Uiso 0.5 1 calc PR . .
C16 C 0.31467(18) 0.06592(8) 0.08975(13) 0.0191(3) Uani 1 1 d . . .
H16A H 0.3671 0.0912 0.1553 0.023 Uiso 1 1 calc R . .
H16B H 0.3992 0.0516 0.0568 0.023 Uiso 1 1 calc R . .
C17 C 0.23631(19) 0.01020(7) 0.12583(13) 0.0185(3) Uani 1 1 d . . .
H17A H 0.1577 -0.0078 0.0605 0.022 Uiso 1 1 calc R . .
H17B H 0.3197 -0.0214 0.1559 0.022 Uiso 1 1 calc R . .
C21 C 0.07319(19) -0.03183(7) 0.23489(13) 0.0184(3) Uani 1 1 d . . .
H21A H 0.1505 -0.0666 0.2473 0.022 Uiso 1 1 calc R . .
H21B H -0.0181 -0.0422 0.1702 0.022 Uiso 1 1 calc R . .
C22 C 0.01213(18) -0.02462(8) 0.33517(13) 0.0212(3) Uani 1 1 d . . .
H22A H -0.0525 0.0137 0.3277 0.025 Uiso 1 1 calc R . .
H22B H -0.0588 -0.0599 0.3388 0.025 Uiso 1 1 calc R . .
C23 C 0.4602(2) 0.06726(10) 0.60927(16) 0.0333(4) Uani 1 1 d . . .
H23A H 0.4424 0.1044 0.563 0.05 Uiso 0.5 1 calc PR . .
H23B H 0.5691 0.0516 0.6178 0.05 Uiso 0.5 1 calc PR . .
H23C H 0.4477 0.0775 0.6819 0.05 Uiso 0.5 1 calc PR . .
H23D H 0.5304 0.0513 0.6788 0.05 Uiso 0.5 1 calc PR . .
H23E H 0.4038 0.1041 0.624 0.05 Uiso 0.5 1 calc PR . .
H23F H 0.5251 0.0782 0.5599 0.05 Uiso 0.5 1 calc PR . .
C24 C 0.3404(2) 0.01891(8) 0.55603(13) 0.0243(3) Uani 1 1 d . . .
C25 C 0.3198(2) -0.04109(9) 0.59210(14) 0.0287(4) Uani 1 1 d . . .
H25 H 0.3821 -0.0605 0.6577 0.034 Uiso 1 1 calc R . .
C26 C 0.1921(2) -0.06606(8) 0.51384(14) 0.0251(4) Uani 1 1 d . . .
C27 C 0.1114(2) -0.12757(10) 0.5068(2) 0.0388(5) Uani 1 1 d . . .
H27A H 0.0224 -0.1297 0.4388 0.058 Uiso 0.5 1 calc PR . .
H27B H 0.0696 -0.133 0.5705 0.058 Uiso 0.5 1 calc PR . .
H27C H 0.1891 -0.1604 0.5063 0.058 Uiso 0.5 1 calc PR . .
H27D H 0.165 -0.1523 0.5716 0.058 Uiso 0.5 1 calc PR . .
H27E H 0.1178 -0.149 0.4399 0.058 Uiso 0.5 1 calc PR . .
H27F H -0.0017 -0.1217 0.5041 0.058 Uiso 0.5 1 calc PR . .
N11 N 0.04994(15) 0.11607(6) 0.01987(10) 0.0146(2) Uani 1 1 d . . .
N12 N 0.20059(15) 0.10446(6) 0.00984(11) 0.0155(2) Uani 1 1 d . . .
N21 N 0.15264(15) 0.02482(6) 0.21051(10) 0.0157(2) Uani 1 1 d . . .
H21 H 0.2314 0.0355 0.2747 0.019 Uiso 1 1 calc R . .
N22 N 0.14206(16) -0.02190(6) 0.43636(11) 0.0199(3) Uani 1 1 d . . .
N23 N 0.23186(16) 0.03081(6) 0.46040(11) 0.0214(3) Uani 1 1 d . . .
Cl2 Cl -0.25877(4) 0.059874(19) 0.12223(3) 0.02186(9) Uani 1 1 d . . .
Zn1 Zn -0.00710(2) 0.101371(8) 0.167595(14) 0.01481(6) 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 0 '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'
Cl Cl 0.1484 0.1585 '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'
K K 0.2009 0.2494 '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 C1 Zn1 107.35(11) . . ?
C3 C2 C5 115.95(16) . . ?
C3 C2 C1 121.20(16) . . ?
C5 C2 C1 122.67(16) . . ?
C2 C3 C4 122.18(16) . . ?
C7 C4 C3 121.56(16) . . ?
C2 C5 C6 121.87(16) . . ?
C7 C6 C5 121.45(16) . . ?
C6 C7 C4 116.93(16) . . ?
C6 C7 C8 121.43(17) . . ?
C4 C7 C8 121.64(17) . . ?
N11 C12 C13 109.97(13) . . ?
N11 C12 C11 120.60(14) . . ?
C13 C12 C11 129.43(14) . . ?
C14 C13 C12 106.55(14) . . ?
N12 C14 C13 106.26(13) . . ?
N12 C14 C15 122.91(15) . . ?
C13 C14 C15 130.82(15) . . ?
N12 C16 C17 112.87(12) . . ?
N21 C17 C16 113.52(13) . . ?
N21 C21 C22 112.51(13) . . ?
N22 C22 C21 112.03(13) . . ?
N23 C24 C25 110.60(16) . . ?
N23 C24 C23 119.81(16) . . ?
C25 C24 C23 129.58(16) . . ?
C26 C25 C24 106.32(15) . . ?
N22 C26 C25 105.87(16) . . ?
N22 C26 C27 122.54(17) . . ?
C25 C26 C27 131.57(16) . . ?
C12 N11 N12 105.57(12) . . ?
C12 N11 Zn1 128.45(10) . . ?
N12 N11 Zn1 121.88(9) . . ?
C14 N12 N11 111.63(12) . . ?
C14 N12 C16 127.04(13) . . ?
N11 N12 C16 121.19(12) . . ?
C21 N21 C17 108.93(12) . . ?
C21 N21 Zn1 112.91(9) . . ?
C17 N21 Zn1 113.39(9) . . ?
C26 N22 N23 112.55(14) . . ?
C26 N22 C22 128.55(15) . . ?
N23 N22 C22 118.88(13) . . ?
C24 N23 N22 104.65(14) . . ?
C1 Zn1 N11 108.69(6) . . ?
C1 Zn1 N21 112.93(7) . . ?
N11 Zn1 N21 92.55(5) . . ?
C1 Zn1 Cl2 125.46(6) . . ?
N11 Zn1 Cl2 106.71(4) . . ?
N21 Zn1 Cl2 105.41(4) . . ?
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
C1 C2 1.502(2) . ?
C1 Zn1 2.0182(17) . ?
C2 C3 1.393(2) . ?
C2 C5 1.401(2) . ?
C3 C4 1.395(2) . ?
C4 C7 1.393(2) . ?
C5 C6 1.402(3) . ?
C6 C7 1.388(3) . ?
C7 C8 1.516(2) . ?
C11 C12 1.501(2) . ?
C12 N11 1.333(2) . ?
C12 C13 1.401(2) . ?
C13 C14 1.376(2) . ?
C14 N12 1.348(2) . ?
C14 C15 1.498(2) . ?
C16 N12 1.4594(19) . ?
C16 C17 1.516(2) . ?
C17 N21 1.4877(19) . ?
C21 N21 1.4808(19) . ?
C21 C22 1.514(2) . ?
C22 N22 1.447(2) . ?
C23 C24 1.494(3) . ?
C24 N23 1.331(2) . ?
C24 C25 1.404(3) . ?
C25 C26 1.371(3) . ?
C26 N22 1.349(2) . ?
C26 C27 1.495(3) . ?
N11 N12 1.3714(17) . ?
N11 Zn1 2.0876(14) . ?
N21 Zn1 2.1290(13) . ?
N22 N23 1.366(2) . ?
Cl2 Zn1 2.2789(6) . ?
