#------------------------------------------------------------------------------
#$Date: 2017-06-28 06:22:16 +0300 (Wed, 28 Jun 2017) $
#$Revision: 198190 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/34/7043466.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_7043466
loop_
_publ_author_name
'Bai, Jianliang'
'Xiao, Xia'
'Zhang, Yue'
'Chao, Jianbin'
'Chen, Xia'
_publ_section_title
;
 β-Pyridylenolate zinc catalysts for the ring-opening homo- and
 copolymerization of ε-caprolactone and lactides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01877K
_journal_year                    2017
_chemical_formula_sum            'C32 H34 N2 O2 Zn2'
_chemical_formula_weight         609.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-23 deposited with the CCDC.
2017-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                109.661(4)
_cell_angle_beta                 104.640(4)
_cell_angle_gamma                108.913(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6494(10)
_cell_length_b                   9.7141(12)
_cell_length_c                   10.1944(13)
_cell_measurement_reflns_used    7382
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.3295
_cell_measurement_theta_min      3.575
_cell_volume                     697.30(15)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10052
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.356
_diffrn_reflns_theta_min         3.617
_exptl_absorpt_coefficient_mu    1.752
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0204P)²+0.6564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3117
_reflns_number_total             3454
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01877k2.cif
_cod_data_source_block           a
_cod_database_code               7043466
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.721
_shelx_estimated_absorpt_t_max   0.779
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Zn1 Zn 0.14242(3) 0.18145(3) 0.57982(2) 0.02166(7) Uani 1 1 d . .
N1 N 0.37705(19) 0.16073(18) 0.62763(17) 0.0219(3) Uani 1 1 d . .
C2 C 0.3062(2) 0.0151(2) 0.7762(2) 0.0231(4) Uani 1 1 d . .
H6 H 0.3581 -0.0122 0.8516 0.028 Uiso 1 1 calc R U
C10 C 0.0221(2) -0.1314(2) 0.79083(19) 0.0196(3) Uani 1 1 d . .
C1 C 0.4281(2) 0.0994(2) 0.7232(2) 0.0212(3) Uani 1 1 d . .
C11 C -0.1318(2) -0.1203(2) 0.8002(2) 0.0236(4) Uani 1 1 d . .
H13 H -0.1682 -0.0506 0.7679 0.028 Uiso 1 1 calc R U
C3 C 0.1281(2) -0.0303(2) 0.73337(19) 0.0189(3) Uani 1 1 d . .
C15 C 0.0690(3) -0.2382(2) 0.8353(2) 0.0262(4) Uani 1 1 d . .
H9 H 0.1720 -0.2498 0.8283 0.031 Uiso 1 1 calc R U
C6 C 0.6035(2) 0.1157(2) 0.7712(2) 0.0282(4) Uani 1 1 d . .
H2 H 0.6412 0.0767 0.8411 0.034 Uiso 1 1 calc R U
C14 C -0.0338(3) -0.3278(2) 0.8898(2) 0.0306(4) Uani 1 1 d . .
H10 H 0.0000 -0.4004 0.9190 0.037 Uiso 1 1 calc R U
C12 C -0.2325(3) -0.2094(2) 0.8560(2) 0.0283(4) Uani 1 1 d . .
H12 H -0.3361 -0.1986 0.8624 0.034 Uiso 1 1 calc R U
C13 C -0.1847(3) -0.3140(2) 0.9027(2) 0.0286(4) Uani 1 1 d . .
C9 C 0.4947(3) 0.2308(2) 0.5768(2) 0.0281(4) Uani 1 1 d . .
H5 H 0.4573 0.2725 0.5093 0.034 Uiso 1 1 calc R U
C7 C 0.7207(3) 0.1875(3) 0.7175(3) 0.0330(5) Uani 1 1 d . .
H3 H 0.8385 0.1973 0.7493 0.040 Uiso 1 1 calc R U
C8 C 0.6653(3) 0.2452(3) 0.6170(2) 0.0316(4) Uani 1 1 d . .
H4 H 0.7429 0.2936 0.5769 0.038 Uiso 1 1 calc R U
C16 C -0.2939(3) -0.4093(3) 0.9647(3) 0.0410(5) Uani 1 1 d . .
H14A H -0.3012 -0.3335 1.0523 0.062 Uiso 1 1 calc R U
H14B H -0.2369 -0.4716 0.9967 0.062 Uiso 1 1 calc R U
H14C H -0.4147 -0.4848 0.8852 0.062 Uiso 1 1 calc R U
O1 O 0.03377(16) 0.00954(15) 0.64060(14) 0.0216(3) Uani 1 1 d . .
C4 C 0.1396(3) 0.3934(3) 0.6208(3) 0.0360(5) Uani 1 1 d . .
H15A H 0.0210 0.3728 0.5539 0.043 Uiso 1 1 calc R U
H15B H 0.1539 0.4472 0.7276 0.043 Uiso 1 1 calc R U
C5 C 0.2823(3) 0.5106(3) 0.5972(3) 0.0489(6) Uani 1 1 d . .
H16A H 0.4002 0.5260 0.6570 0.073 Uiso 1 1 calc R U
H16B H 0.2787 0.6162 0.6304 0.073 Uiso 1 1 calc R U
H16C H 0.2601 0.4654 0.4889 0.073 Uiso 1 1 calc R U
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'
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
C4 Zn1 O1 131.82(7) . .
C4 Zn1 N1 121.87(8) . .
O1 Zn1 N1 91.64(5) . .
C4 Zn1 O1 115.03(8) . 2_556
O1 Zn1 O1 82.16(5) . 2_556
N1 Zn1 O1 106.09(6) . 2_556
C4 Zn1 Zn1 135.95(7) . 2_556
O1 Zn1 Zn1 42.31(4) . 2_556
N1 Zn1 Zn1 101.93(4) . 2_556
O1 Zn1 Zn1 39.85(3) 2_556 2_556
C9 N1 C1 118.78(16) . .
C9 N1 Zn1 117.63(13) . .
C1 N1 Zn1 123.03(12) . .
C3 C2 C1 129.18(16) . .
C11 C10 C15 117.93(16) . .
C11 C10 C3 119.03(16) . .
C15 C10 C3 123.04(16) . .
N1 C1 C6 119.46(16) . .
N1 C1 C2 121.83(16) . .
C6 C1 C2 118.71(16) . .
C12 C11 C10 121.09(17) . .
O1 C3 C2 124.83(16) . .
O1 C3 C10 114.37(15) . .
C2 C3 C10 120.80(15) . .
C14 C15 C10 120.44(18) . .
C7 C6 C1 120.54(18) . .
C13 C14 C15 121.69(18) . .
C11 C12 C13 121.13(19) . .
C14 C13 C12 117.70(17) . .
C14 C13 C16 121.44(19) . .
C12 C13 C16 120.9(2) . .
N1 C9 C8 123.75(18) . .
C8 C7 C6 119.32(18) . .
C9 C8 C7 118.09(18) . .
C3 O1 Zn1 124.13(11) . .
C3 O1 Zn1 115.90(11) . 2_556
Zn1 O1 Zn1 97.84(5) . 2_556
C5 C4 Zn1 115.28(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 C4 1.968(2) .
Zn1 O1 2.0073(12) .
Zn1 N1 2.0561(15) .
Zn1 O1 2.1082(13) 2_556
Zn1 Zn1 3.1029(6) 2_556
N1 C9 1.350(2) .
N1 C1 1.358(2) .
C2 C3 1.360(2) .
C2 C1 1.449(2) .
C10 C11 1.394(3) .
C10 C15 1.394(2) .
C10 C3 1.491(2) .
C1 C6 1.408(2) .
C11 C12 1.387(3) .
C3 O1 1.331(2) .
C15 C14 1.389(3) .
C6 C7 1.375(3) .
C14 C13 1.388(3) .
C12 C13 1.389(3) .
C13 C16 1.510(3) .
C9 C8 1.374(3) .
C7 C8 1.381(3) .
O1 Zn1 2.1082(13) 2_556
C4 C5 1.517(3) .
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_4
C9 N1 C1 C6 2.3(3) .
Zn1 N1 C1 C6 -168.83(14) .
C9 N1 C1 C2 -176.82(17) .
Zn1 N1 C1 C2 12.0(2) .
C3 C2 C1 N1 6.9(3) .
C3 C2 C1 C6 -172.28(19) .
C15 C10 C11 C12 1.7(3) .
C3 C10 C11 C12 -178.63(17) .
C1 C2 C3 O1 -6.6(3) .
C1 C2 C3 C10 173.84(18) .
C11 C10 C3 O1 -26.1(2) .
C15 C10 C3 O1 153.54(17) .
C11 C10 C3 C2 153.53(18) .
C15 C10 C3 C2 -26.8(3) .
C11 C10 C15 C14 -1.2(3) .
C3 C10 C15 C14 179.19(17) .
N1 C1 C6 C7 -2.4(3) .
C2 C1 C6 C7 176.74(19) .
C10 C15 C14 C13 -0.4(3) .
C10 C11 C12 C13 -0.7(3) .
C15 C14 C13 C12 1.3(3) .
C15 C14 C13 C16 -178.9(2) .
C11 C12 C13 C14 -0.8(3) .
C11 C12 C13 C16 179.40(19) .
C1 N1 C9 C8 -0.5(3) .
Zn1 N1 C9 C8 171.12(17) .
C1 C6 C7 C8 0.7(3) .
N1 C9 C8 C7 -1.3(3) .
C6 C7 C8 C9 1.1(3) .
C2 C3 O1 Zn1 -13.2(2) .
C10 C3 O1 Zn1 166.36(11) .
C2 C3 O1 Zn1 107.58(18) 2_556
C10 C3 O1 Zn1 -72.83(16) 2_556
