#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:58:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178675 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/86/4078685.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_4078685
loop_
_publ_author_name
'Petrus, Rafał'
'Sobota, Piotr'
_publ_section_title
;
 Zinc Complexes Supported by Maltolato Ligands: Synthesis, Structure,
 Solution Behavior, and Application in Ring-Opening Polymerization of
 Lactides
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4755
_journal_paper_doi               10.1021/om300321h
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C24 H20 O12 Zn2, 2(C H2 Cl2)'
_chemical_formula_sum            'C26 H24 Cl4 O12 Zn2'
_chemical_formula_weight         801.03
_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                100.83(2)
_cell_angle_beta                 96.86(3)
_cell_angle_gamma                106.80(3)
_cell_formula_units_Z            1
_cell_length_a                   7.469(3)
_cell_length_b                   7.740(4)
_cell_length_c                   14.296(6)
_cell_measurement_reflns_used    4102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.8375
_cell_measurement_theta_min      2.8502
_cell_volume                     763.7(6)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'KUMA KM4 CCD κ-geometry diffractometer'
_diffrn_measurement_method       ω
_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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11285
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.921
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0569
_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)+(0.0911P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1468
_reflns_number_gt                2685
_reflns_number_total             3942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300321h_si_002.cif
_cod_data_source_block           compound_{1a}2
_cod_database_code               4078685
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
Zn1 Zn 0.40738(6) 0.49888(6) 0.39703(4) 0.02207(16) Uani 1 1 d .
O1 O 0.1266(4) 0.4384(4) 0.4056(2) 0.0282(6) Uani 1 1 d .
C1 C 0.0288(6) 0.3953(6) 0.3218(4) 0.0308(10) Uani 1 1 d .
C2 C 0.1191(6) 0.3739(6) 0.2405(3) 0.0316(10) Uani 1 1 d .
O2 O 0.3061(5) 0.4008(5) 0.2544(2) 0.0356(7) Uani 1 1 d .
C3 C 0.0115(7) 0.3262(7) 0.1480(4) 0.0422(12) Uani 1 1 d .
O3 O -0.1797(5) 0.3005(5) 0.1345(3) 0.0433(9) Uani 1 1 d .
C4 C -0.2646(7) 0.3255(8) 0.2138(4) 0.0467(13) Uani 1 1 d .
H4 H -0.3967 0.3106 0.2028 0.056 Uiso 1 1 calc R
C5 C -0.1748(6) 0.3683(6) 0.3031(4) 0.0357(11) Uani 1 1 d .
H5 H -0.2412 0.3817 0.3553 0.043 Uiso 1 1 calc R
C6 C 0.0795(9) 0.2924(10) 0.0571(4) 0.0609(17) Uani 1 1 d .
H6A H -0.0255 0.2066 0.0066 0.091 Uiso 1 1 calc R
H6B H 0.1819 0.2379 0.0655 0.091 Uiso 1 1 calc R
H6C H 0.1278 0.4100 0.0379 0.091 Uiso 1 1 calc R
O7 O 0.6122(4) 0.7111(4) 0.3724(2) 0.0251(6) Uani 1 1 d .
C7 C 0.6772(5) 0.8512(5) 0.4436(3) 0.0216(8) Uani 1 1 d .
C8 C 0.6230(5) 0.8412(5) 0.5362(3) 0.0225(8) Uani 1 1 d .
O8 O 0.5012(4) 0.6795(4) 0.5412(2) 0.0217(6) Uani 1 1 d .
C9 C 0.6905(5) 0.9939(6) 0.6115(3) 0.0254(9) Uani 1 1 d .
O9 O 0.8102(4) 1.1573(4) 0.6000(2) 0.0274(6) Uani 1 1 d .
C10 C 0.8623(6) 1.1680(6) 0.5143(3) 0.0287(9) Uani 1 1 d .
H10 H 0.9448 1.2830 0.5083 0.034 Uiso 1 1 calc R
C11 C 0.8039(6) 1.0251(6) 0.4365(3) 0.0265(9) Uani 1 1 d .
H11 H 0.8460 1.0387 0.3774 0.032 Uiso 1 1 calc R
C12 C 0.6471(6) 1.0088(6) 0.7113(3) 0.0312(10) Uani 1 1 d .
H12A H 0.5107 0.9895 0.7084 0.047 Uiso 1 1 calc R
H12B H 0.7200 1.1324 0.7515 0.047 Uiso 1 1 calc R
H12C H 0.6819 0.9144 0.7394 0.047 Uiso 1 1 calc R
C13 C 0.3778(7) 0.3074(7) 0.8586(4) 0.0414(12) Uani 1 1 d .
H13A H 0.3646 0.4259 0.8922 0.050 Uiso 1 1 calc R
H13B H 0.4376 0.3291 0.8019 0.050 Uiso 1 1 calc R
Cl14 Cl 0.1510(2) 0.1398(3) 0.81892(11) 0.0677(5) Uani 1 1 d .
Cl15 Cl 0.5254(2) 0.2357(2) 0.93794(10) 0.0559(4) 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 0.0000 0.0000 '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'
Zn Zn 0.2839 1.4301 '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'
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
O8 Zn1 O2 113.11(13) 2_666 .
O8 Zn1 O7 115.64(12) 2_666 .
O2 Zn1 O7 91.00(13) . .
O8 Zn1 O1 105.66(11) 2_666 .
O2 Zn1 O1 83.41(13) . .
O7 Zn1 O1 136.95(12) . .
O8 Zn1 O8 84.28(12) 2_666 .
O2 Zn1 O8 162.54(12) . .
O7 Zn1 O8 79.44(11) . .
O1 Zn1 O8 93.57(12) . .
O8 Zn1 Zn1 44.20(8) 2_666 2_666
O2 Zn1 Zn1 157.27(10) . 2_666
O7 Zn1 Zn1 98.72(9) . 2_666
O1 Zn1 Zn1 102.61(10) . 2_666
O8 Zn1 Zn1 40.09(8) . 2_666
C1 O1 Zn1 109.5(3) . .
O1 C1 C2 119.2(4) . .
O1 C1 C5 123.3(4) . .
C2 C1 C5 117.5(4) . .
O2 C2 C3 121.2(4) . .
O2 C2 C1 119.4(4) . .
C3 C2 C1 119.3(4) . .
C2 O2 Zn1 107.4(3) . .
O3 C3 C2 120.8(5) . .
O3 C3 C6 112.6(5) . .
C2 C3 C6 126.5(5) . .
C3 O3 C4 119.3(4) . .
C5 C4 O3 123.9(5) . .
C5 C4 H4 118.0 . .
O3 C4 H4 118.0 . .
C4 C5 C1 119.1(5) . .
C4 C5 H5 120.4 . .
C1 C5 H5 120.4 . .
C3 C6 H6A 109.5 . .
C3 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C3 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C7 O7 Zn1 114.2(2) . .
O7 C7 C11 122.8(4) . .
O7 C7 C8 120.4(3) . .
C11 C7 C8 116.9(4) . .
O8 C8 C9 123.9(4) . .
O8 C8 C7 116.3(3) . .
C9 C8 C7 119.8(4) . .
C8 O8 Zn1 120.8(2) . 2_666
C8 O8 Zn1 108.8(2) . .
Zn1 O8 Zn1 95.72(12) 2_666 .
C8 C9 O9 120.7(4) . .
C8 C9 C12 126.8(4) . .
O9 C9 C12 112.5(3) . .
C10 O9 C9 120.1(3) . .
C11 C10 O9 123.4(4) . .
C11 C10 H10 118.3 . .
O9 C10 H10 118.3 . .
C10 C11 C7 119.2(4) . .
C10 C11 H11 120.4 . .
C7 C11 H11 120.4 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Cl14 C13 Cl15 111.4(3) . .
Cl14 C13 H13A 109.4 . .
Cl15 C13 H13A 109.4 . .
Cl14 C13 H13B 109.4 . .
Cl15 C13 H13B 109.4 . .
H13A C13 H13B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O8 2.003(3) 2_666
Zn1 O2 2.006(3) .
Zn1 O7 2.014(3) .
Zn1 O1 2.037(3) .
Zn1 O8 2.168(3) .
Zn1 Zn1 3.0945(16) 2_666
O1 C1 1.256(6) .
C1 C2 1.419(7) .
C1 C5 1.458(6) .
C2 O2 1.336(5) .
C2 C3 1.385(7) .
C3 O3 1.368(6) .
C3 C6 1.457(8) .
O3 C4 1.373(7) .
C4 C5 1.303(8) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
O7 C7 1.269(5) .
C7 C11 1.434(5) .
C7 C8 1.439(6) .
C8 O8 1.338(5) .
C8 C9 1.363(6) .
O8 Zn1 2.003(3) 2_666
C9 O9 1.373(5) .
C9 C12 1.491(6) .
O9 C10 1.340(5) .
C10 C11 1.339(6) .
C10 H10 0.9500 .
C11 H11 0.9500 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 Cl14 1.760(5) .
C13 Cl15 1.761(5) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5 O8 0.95 2.57 3.481(6) 160.9 2_566
C10 H10 O1 0.95 2.38 3.202(5) 145.3 1_665
C12 H12C O2 0.98 2.48 3.406(6) 156.6 2_666
C13 H13B O7 0.99 2.42 3.289(6) 146.1 2_666
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O8 Zn1 O1 C1 -121.0(3) 2_666 .
O2 Zn1 O1 C1 -8.8(3) . .
O7 Zn1 O1 C1 75.6(3) . .
O8 Zn1 O1 C1 154.0(3) . .
Zn1 Zn1 O1 C1 -166.5(2) 2_666 .
Zn1 O1 C1 C2 7.5(4) . .
Zn1 O1 C1 C5 -171.6(3) . .
O1 C1 C2 O2 -0.4(6) . .
C5 C1 C2 O2 178.8(4) . .
O1 C1 C2 C3 179.9(4) . .
C5 C1 C2 C3 -0.9(6) . .
C3 C2 O2 Zn1 172.7(4) . .
C1 C2 O2 Zn1 -7.0(5) . .
O8 Zn1 O2 C2 112.5(3) 2_666 .
O7 Zn1 O2 C2 -129.0(3) . .
O1 Zn1 O2 C2 8.2(3) . .
O8 Zn1 O2 C2 -72.7(5) . .
Zn1 Zn1 O2 C2 115.3(3) 2_666 .
O2 C2 C3 O3 -179.5(4) . .
C1 C2 C3 O3 0.3(7) . .
O2 C2 C3 C6 2.6(8) . .
C1 C2 C3 C6 -177.7(5) . .
C2 C3 O3 C4 1.1(7) . .
C6 C3 O3 C4 179.3(5) . .
C3 O3 C4 C5 -1.9(7) . .
O3 C4 C5 C1 1.2(8) . .
O1 C1 C5 C4 179.4(4) . .
C2 C1 C5 C4 0.3(7) . .
O8 Zn1 O7 C7 -86.9(3) 2_666 .
O2 Zn1 O7 C7 156.8(3) . .
O1 Zn1 O7 C7 75.3(3) . .
O8 Zn1 O7 C7 -8.5(3) . .
Zn1 Zn1 O7 C7 -43.9(3) 2_666 .
Zn1 O7 C7 C11 -171.1(3) . .
Zn1 O7 C7 C8 8.1(4) . .
O7 C7 C8 O8 -0.8(5) . .
C11 C7 C8 O8 178.5(3) . .
O7 C7 C8 C9 -178.5(4) . .
C11 C7 C8 C9 0.7(5) . .
C9 C8 O8 Zn1 -79.6(4) . 2_666
C7 C8 O8 Zn1 102.7(3) . 2_666
C9 C8 O8 Zn1 171.5(3) . .
C7 C8 O8 Zn1 -6.2(4) . .
O8 Zn1 O8 C8 125.3(3) 2_666 .
O2 Zn1 O8 C8 -50.0(5) . .
O7 Zn1 O8 C8 7.8(2) . .
O1 Zn1 O8 C8 -129.3(2) . .
Zn1 Zn1 O8 C8 125.3(3) 2_666 .
O8 Zn1 O8 Zn1 0.0 2_666 2_666
O2 Zn1 O8 Zn1 -175.2(3) . 2_666
O7 Zn1 O8 Zn1 -117.45(12) . 2_666
O1 Zn1 O8 Zn1 105.40(12) . 2_666
O8 C8 C9 O9 -177.8(3) . .
C7 C8 C9 O9 -0.2(6) . .
O8 C8 C9 C12 1.5(6) . .
C7 C8 C9 C12 179.1(4) . .
C8 C9 O9 C10 -0.1(5) . .
C12 C9 O9 C10 -179.4(3) . .
C9 O9 C10 C11 -0.3(6) . .
O9 C10 C11 C7 0.9(6) . .
O7 C7 C11 C10 178.2(4) . .
C8 C7 C11 C10 -1.1(6) . .
