#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:58:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179272 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/92/4319277.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_4319277
loop_
_publ_author_name
'Donald J. Darensbourg'
'Patrick Rainey'
'Jason Yarbrough'
_publ_section_title
;
 Bis-Salicylaldiminato Complexes of Zinc. Examination of the Catalyzed
 Epoxide/CO2 Copolymerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              986
_journal_page_last               993
_journal_paper_doi               10.1021/ic0006403
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C38 H40 Cl4 N2 O2 Zn'
_chemical_formula_weight         763.94
_chemical_name_systematic
;
 ?
;
_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                 110.4660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.7086(16)
_cell_length_b                   17.3307(14)
_cell_length_c                   22.5847(18)
_cell_measurement_temperature    110(2)
_cell_volume                     7227.2(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16077
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.017
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3360
_refine_diff_density_max         2.609
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0622
_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)+(0.1045P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1601
_reflns_number_gt                3959
_reflns_number_total             5213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0006403_1.cif
_cod_data_source_block           ddprm
_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               4319277
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
Zn1 Zn 0.23360(2) 0.78660(3) 0.19949(2) 0.0224(2) Uani 1 1 d . . .
O1 O 0.30010(15) 0.71755(16) 0.17921(13) 0.0244(7) Uani 1 1 d . . .
O2 O 0.24308(15) 0.78084(16) 0.28822(13) 0.0236(7) Uani 1 1 d . . .
N1 N 0.27428(18) 0.88274(19) 0.17564(15) 0.0238(8) Uani 1 1 d . . .
N2 N 0.12918(17) 0.7519(2) 0.16786(15) 0.0218(8) Uani 1 1 d . . .
Cl1 Cl 0.07394(7) 0.58261(8) 0.39659(6) 0.0473(4) Uani 1 1 d . . .
Cl2 Cl 0.58450(5) 0.79828(6) 0.16681(5) 0.0264(3) Uani 1 1 d . . .
Cl3 Cl 0.29724(6) 0.77728(7) 0.42561(5) 0.0338(3) Uani 1 1 d . . .
Cl4 Cl 0.39071(6) 0.58565(6) 0.17572(6) 0.0333(3) Uani 1 1 d . . .
C1 C 0.3609(2) 0.7384(3) 0.17389(18) 0.0230(10) Uani 1 1 d . . .
C2 C 0.4126(2) 0.6823(2) 0.17239(18) 0.0234(10) Uani 1 1 d . . .
C3 C 0.4793(2) 0.6998(2) 0.17015(19) 0.0244(10) Uani 1 1 d . . .
H3 H 0.5114 0.6606 0.1700 0.029 Uiso 1 1 calc R . .
C4 C 0.4990(2) 0.7770(2) 0.16808(18) 0.0221(10) Uani 1 1 d . . .
C5 C 0.4503(2) 0.8343(2) 0.16656(18) 0.0237(10) Uani 1 1 d . . .
H5 H 0.4632 0.8855 0.1641 0.028 Uiso 1 1 calc R . .
C6 C 0.3814(2) 0.8173(2) 0.16865(17) 0.0205(9) Uani 1 1 d . . .
C7 C 0.3356(2) 0.8818(2) 0.16721(17) 0.0230(10) Uani 1 1 d . . .
H7 H 0.3523 0.9294 0.1591 0.028 Uiso 1 1 calc R . .
C8 C 0.2409(2) 0.9592(2) 0.1714(2) 0.0229(10) Uani 1 1 d . . .
C9 C 0.2025(2) 0.9914(2) 0.11225(19) 0.0271(10) Uani 1 1 d . . .
C10 C 0.1708(2) 1.0628(3) 0.1121(2) 0.0293(10) Uani 1 1 d . . .
H10 H 0.1451 1.0858 0.0736 0.035 Uiso 1 1 calc R . .
C11 C 0.1760(2) 1.1010(3) 0.1669(2) 0.0286(10) Uani 1 1 d . . .
H11 H 0.1534 1.1485 0.1651 0.034 Uiso 1 1 calc R . .
C12 C 0.2153(2) 1.0681(2) 0.2247(2) 0.0267(10) Uani 1 1 d . . .
H12 H 0.2195 1.0946 0.2616 0.032 Uiso 1 1 calc R . .
C13 C 0.2485(2) 0.9967(2) 0.22883(19) 0.0237(10) Uani 1 1 d . . .
C14 C 0.2944(2) 0.9634(3) 0.2918(2) 0.0291(11) Uani 1 1 d . . .
H14 H 0.3004 0.9082 0.2854 0.035 Uiso 1 1 calc R . .
C15 C 0.2609(2) 0.9707(3) 0.3427(2) 0.0335(11) Uani 1 1 d . . .
H15A H 0.2571 1.0242 0.3519 0.050 Uiso 1 1 calc R . .
H15B H 0.2910 0.9447 0.3802 0.050 Uiso 1 1 calc R . .
H15C H 0.2136 0.9478 0.3281 0.050 Uiso 1 1 calc R . .
C16 C 0.3703(2) 1.0003(3) 0.3136(2) 0.0325(11) Uani 1 1 d . . .
H16A H 0.3914 0.9933 0.2816 0.049 Uiso 1 1 calc R . .
H16B H 0.4005 0.9762 0.3521 0.049 Uiso 1 1 calc R . .
H16C H 0.3664 1.0545 0.3208 0.049 Uiso 1 1 calc R . .
C17 C 0.1953(2) 0.9527(3) 0.0501(2) 0.0325(11) Uani 1 1 d . . .
H17 H 0.2212 0.9034 0.0596 0.039 Uiso 1 1 calc R . .
C18 C 0.1152(2) 0.9359(3) 0.0102(2) 0.0369(12) Uani 1 1 d . . .
H18A H 0.0940 0.9046 0.0343 0.055 Uiso 1 1 calc R . .
H18B H 0.1127 0.9090 -0.0276 0.055 Uiso 1 1 calc R . .
H18C H 0.0891 0.9836 -0.0007 0.055 Uiso 1 1 calc R . .
C19 C 0.2289(3) 1.0016(3) 0.0108(2) 0.0399(12) Uani 1 1 d . . .
H19A H 0.2044 1.0503 0.0010 0.060 Uiso 1 1 calc R . .
H19B H 0.2242 0.9749 -0.0277 0.060 Uiso 1 1 calc R . .
H19C H 0.2793 1.0101 0.0345 0.060 Uiso 1 1 calc R . .
C20 C 0.2033(2) 0.7380(2) 0.31030(19) 0.0245(10) Uani 1 1 d . . .
C21 C 0.2209(2) 0.7289(2) 0.37675(19) 0.0250(10) Uani 1 1 d . . .
C22 C 0.1832(2) 0.6831(3) 0.4030(2) 0.0302(11) Uani 1 1 d . . .
H22 H 0.1977 0.6782 0.4467 0.036 Uiso 1 1 calc R . .
C23 C 0.1225(2) 0.6432(3) 0.3638(2) 0.0322(11) Uani 1 1 d . . .
C24 C 0.1013(2) 0.6510(3) 0.2999(2) 0.0315(11) Uani 1 1 d . . .
H24 H 0.0612 0.6236 0.2742 0.038 Uiso 1 1 calc R . .
C25 C 0.1388(2) 0.6998(2) 0.27165(19) 0.0230(10) Uani 1 1 d . . .
C26 C 0.1051(2) 0.7129(2) 0.2055(2) 0.0252(10) Uani 1 1 d . . .
H26 H 0.0598 0.6905 0.1867 0.030 Uiso 1 1 calc R . .
C27 C 0.0757(2) 0.7676(3) 0.10591(19) 0.0269(10) Uani 1 1 d . . .
C28 C 0.0814(2) 0.7290(3) 0.0533(2) 0.0283(11) Uani 1 1 d . . .
C29 C 0.0296(2) 0.7453(3) -0.0056(2) 0.0321(11) Uani 1 1 d . . .
H29 H 0.0325 0.7210 -0.0414 0.039 Uiso 1 1 calc R . .
C30 C -0.0253(2) 0.7962(3) -0.0117(2) 0.0347(12) Uani 1 1 d . . .
H30 H -0.0595 0.8061 -0.0514 0.042 Uiso 1 1 calc R . .
C31 C -0.0303(3) 0.8331(3) 0.0408(2) 0.0366(12) Uani 1 1 d . . .
H31 H -0.0682 0.8675 0.0359 0.044 Uiso 1 1 calc R . .
C32 C 0.0199(2) 0.8200(3) 0.1011(2) 0.0296(10) Uani 1 1 d . . .
C33 C 0.0134(2) 0.8648(3) 0.1569(2) 0.0310(11) Uani 1 1 d . . .
H33 H 0.0436 0.8388 0.1957 0.037 Uiso 1 1 calc R . .
C34 C 0.0417(3) 0.9463(3) 0.1583(3) 0.0530(15) Uani 1 1 d . . .
H34A H 0.0130 0.9731 0.1206 0.079 Uiso 1 1 calc R . .
H34B H 0.0912 0.9447 0.1604 0.079 Uiso 1 1 calc R . .
H34C H 0.0389 0.9729 0.1946 0.079 Uiso 1 1 calc R . .
C35 C -0.0629(3) 0.8677(3) 0.1573(2) 0.0430(13) Uani 1 1 d . . .
H35A H -0.0624 0.8874 0.1971 0.064 Uiso 1 1 calc R . .
H35B H -0.0832 0.8167 0.1510 0.064 Uiso 1 1 calc R . .
H35C H -0.0917 0.9009 0.1239 0.064 Uiso 1 1 calc R . .
C36 C 0.1399(2) 0.6690(3) 0.05780(19) 0.0280(10) Uani 1 1 d . . .
H36 H 0.1668 0.6591 0.1026 0.034 Uiso 1 1 calc R . .
C37 C 0.1934(3) 0.7007(3) 0.0279(2) 0.0361(12) Uani 1 1 d . . .
H37A H 0.1684 0.7098 -0.0163 0.054 Uiso 1 1 calc R . .
H37B H 0.2315 0.6639 0.0332 0.054 Uiso 1 1 calc R . .
H37C H 0.2138 0.7482 0.0482 0.054 Uiso 1 1 calc R . .
C38 C 0.1065(3) 0.5931(3) 0.0271(2) 0.0372(12) Uani 1 1 d . . .
H38A H 0.0711 0.5764 0.0446 0.056 Uiso 1 1 calc R . .
H38B H 0.1437 0.5547 0.0351 0.056 Uiso 1 1 calc R . .
H38C H 0.0838 0.6004 -0.0176 0.056 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
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'
O O 0.0106 0.0060 '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'
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
O1 Zn1 O2 112.37(11) . . ?
O1 Zn1 N1 94.73(12) . . ?
O2 Zn1 N1 114.57(12) . . ?
O1 Zn1 N2 114.88(12) . . ?
O2 Zn1 N2 93.90(12) . . ?
N1 Zn1 N2 127.36(14) . . ?
C1 O1 Zn1 124.9(3) . . ?
C20 O2 Zn1 124.8(3) . . ?
C7 N1 C8 115.1(3) . . ?
C7 N1 Zn1 120.9(3) . . ?
C8 N1 Zn1 123.8(3) . . ?
C26 N2 C27 114.8(3) . . ?
C26 N2 Zn1 118.9(3) . . ?
C27 N2 Zn1 126.2(3) . . ?
O1 C1 C2 120.5(4) . . ?
O1 C1 C6 124.5(4) . . ?
C2 C1 C6 115.0(4) . . ?
C3 C2 C1 123.9(4) . . ?
C3 C2 Cl4 118.1(3) . . ?
C1 C2 Cl4 117.9(3) . . ?
C2 C3 C4 119.7(4) . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 Cl2 121.3(3) . . ?
C3 C4 Cl2 119.1(3) . . ?
C4 C5 C6 121.5(4) . . ?
C5 C6 C7 116.5(4) . . ?
C5 C6 C1 120.2(4) . . ?
C7 C6 C1 123.3(4) . . ?
N1 C7 C6 128.7(4) . . ?
C9 C8 C13 122.8(4) . . ?
C9 C8 N1 120.2(4) . . ?
C13 C8 N1 117.0(4) . . ?
C10 C9 C8 116.8(4) . . ?
C10 C9 C17 119.8(4) . . ?
C8 C9 C17 123.5(4) . . ?
C11 C10 C9 122.4(4) . . ?
C10 C11 C12 119.4(4) . . ?
C11 C12 C13 121.7(4) . . ?
C12 C13 C8 116.9(4) . . ?
C12 C13 C14 121.3(4) . . ?
C8 C13 C14 121.8(4) . . ?
C13 C14 C15 113.9(4) . . ?
C13 C14 C16 109.8(4) . . ?
C15 C14 C16 110.7(4) . . ?
C9 C17 C19 111.8(4) . . ?
C9 C17 C18 111.6(4) . . ?
C19 C17 C18 109.0(4) . . ?
O2 C20 C21 120.7(4) . . ?
O2 C20 C25 123.9(4) . . ?
C21 C20 C25 115.4(4) . . ?
C22 C21 C20 123.8(4) . . ?
C22 C21 Cl3 119.3(3) . . ?
C20 C21 Cl3 116.9(3) . . ?
C21 C22 C23 119.4(4) . . ?
C24 C23 C22 120.0(4) . . ?
C24 C23 Cl1 119.8(4) . . ?
C22 C23 Cl1 120.2(3) . . ?
C23 C24 C25 121.5(4) . . ?
C24 C25 C26 116.2(4) . . ?
C24 C25 C20 119.8(4) . . ?
C26 C25 C20 123.8(4) . . ?
N2 C26 C25 128.7(4) . . ?
C32 C27 C28 122.5(4) . . ?
C32 C27 N2 118.8(4) . . ?
C28 C27 N2 118.7(4) . . ?
C29 C28 C27 117.6(4) . . ?
C29 C28 C36 119.0(4) . . ?
C27 C28 C36 123.4(4) . . ?
C30 C29 C28 121.1(4) . . ?
C29 C30 C31 120.4(4) . . ?
C30 C31 C32 121.6(4) . . ?
C31 C32 C27 116.8(4) . . ?
C31 C32 C33 119.2(4) . . ?
C27 C32 C33 123.9(4) . . ?
C35 C33 C34 109.2(4) . . ?
C35 C33 C32 113.2(4) . . ?
C34 C33 C32 110.7(4) . . ?
C38 C36 C28 111.2(4) . . ?
C38 C36 C37 111.2(4) . . ?
C28 C36 C37 110.2(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
Zn1 O1 1.944(3) . ?
Zn1 O2 1.949(3) . ?
Zn1 N1 2.003(3) . ?
Zn1 N2 2.020(3) . ?
O1 C1 1.296(5) . ?
O2 C20 1.299(5) . ?
N1 C7 1.287(5) . ?
N1 C8 1.468(5) . ?
N2 C26 1.298(5) . ?
N2 C27 1.453(5) . ?
Cl1 C23 1.750(4) . ?
Cl2 C4 1.736(4) . ?
Cl3 C21 1.739(4) . ?
Cl4 C2 1.738(4) . ?
C1 C2 1.417(6) . ?
C1 C6 1.443(6) . ?
C2 C3 1.367(6) . ?
C3 C4 1.398(6) . ?
C4 C5 1.373(6) . ?
C5 C6 1.406(5) . ?
C6 C7 1.430(6) . ?
C8 C9 1.399(6) . ?
C8 C13 1.412(6) . ?
C9 C10 1.387(6) . ?
C9 C17 1.516(6) . ?
C10 C11 1.374(6) . ?
C11 C12 1.387(6) . ?
C12 C13 1.387(6) . ?
C13 C14 1.508(6) . ?
C14 C15 1.517(6) . ?
C14 C16 1.541(6) . ?
C17 C19 1.536(6) . ?
C17 C18 1.547(6) . ?
C20 C21 1.426(6) . ?
C20 C25 1.428(6) . ?
C21 C22 1.358(6) . ?
C22 C23 1.396(6) . ?
C23 C24 1.363(6) . ?
C24 C25 1.413(6) . ?
C25 C26 1.425(6) . ?
C27 C32 1.400(6) . ?
C27 C28 1.402(6) . ?
C28 C29 1.394(6) . ?
C28 C36 1.530(6) . ?
C29 C30 1.366(6) . ?
C30 C31 1.381(6) . ?
C31 C32 1.394(6) . ?
C32 C33 1.523(6) . ?
C33 C35 1.507(6) . ?
C33 C34 1.516(7) . ?
C36 C38 1.525(6) . ?
C36 C37 1.538(6) . ?
