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#$Date: 2017-06-28 06:22:16 +0300 (Wed, 28 Jun 2017) $
#$Revision: 198190 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/34/7043468.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_7043468
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 H28 F6 N2 O2 Zn2'
_chemical_formula_weight         717.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 96.454(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0405(6)
_cell_length_b                   11.0680(7)
_cell_length_c                   13.8622(8)
_cell_measurement_reflns_used    7786
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.2525
_cell_measurement_theta_min      2.958
_cell_volume                     1530.72(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14700
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.302
_diffrn_reflns_theta_min         2.958
_exptl_absorpt_coefficient_mu    1.636
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0270P)²+4.5365P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3206
_reflns_number_total             3771
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt01877k2.cif
_cod_data_source_block           1
_cod_database_code               7043468
_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   0.736
_shelx_estimated_absorpt_t_max   0.894
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Zn1 Zn 0.35556(3) 0.94909(3) 0.00221(2) 0.02674(12) Uani 1 1 d . .
O1 O 0.5432(2) 0.9107(2) 0.05955(14) 0.0262(4) Uani 1 1 d . .
C10 C 0.7120(3) 0.8337(3) 0.1783(2) 0.0246(6) Uani 1 1 d . .
C1 C 0.3704(3) 0.9659(3) 0.2224(2) 0.0251(6) Uani 1 1 d . .
C15 C 0.7650(3) 0.7363(3) 0.1300(2) 0.0288(6) Uani 1 1 d . .
C7 C 0.2024(3) 1.0567(3) 0.3096(3) 0.0386(8) Uani 1 1 d . .
H7 H 0.1678 1.0749 0.3690 0.046 Uiso 1 1 calc R U
C9 C 0.1894(3) 1.0664(3) 0.1385(2) 0.0331(7) Uani 1 1 d . .
H9 H 0.1429 1.0913 0.0783 0.040 Uiso 1 1 calc R U
C3 C 0.5750(3) 0.8838(3) 0.1530(2) 0.0240(6) Uani 1 1 d . .
C2 C 0.4975(3) 0.9033(3) 0.2252(2) 0.0276(6) Uani 1 1 d . .
H2 H 0.5313 0.8712 0.2866 0.033 Uiso 1 1 calc R U
C11 C 0.7947(3) 0.8881(3) 0.2535(2) 0.0325(7) Uani 1 1 d . .
H11 H 0.7610 0.9541 0.2873 0.039 Uiso 1 1 calc R U
C4 C 0.2066(3) 0.8683(3) -0.0763(2) 0.0383(8) Uani 1 1 d . .
H4A H 0.1376 0.9294 -0.0981 0.046 Uiso 1 1 calc R U
H4B H 0.2402 0.8341 -0.1350 0.046 Uiso 1 1 calc R U
C12 C 0.9242(3) 0.8490(3) 0.2804(3) 0.0403(8) Uani 1 1 d . .
H12 H 0.9781 0.8876 0.3321 0.048 Uiso 1 1 calc R U
C6 C 0.3180(3) 0.9915(3) 0.3094(2) 0.0332(7) Uani 1 1 d . .
H6 H 0.3632 0.9632 0.3690 0.040 Uiso 1 1 calc R U
C13 C 0.9747(4) 0.7541(4) 0.2323(3) 0.0466(9) Uani 1 1 d . .
H13 H 1.0638 0.7271 0.2504 0.056 Uiso 1 1 calc R U
C8 C 0.1362(3) 1.0960(3) 0.2218(3) 0.0377(7) Uani 1 1 d . .
H8 H 0.0562 1.1422 0.2198 0.045 Uiso 1 1 calc R U
C14 C 0.8956(3) 0.6979(3) 0.1574(3) 0.0394(8) Uani 1 1 d . .
H14 H 0.9310 0.6323 0.1242 0.047 Uiso 1 1 calc R U
N1 N 0.3043(2) 1.0037(2) 0.13699(17) 0.0269(5) Uani 1 1 d . .
F1 F 0.7323(3) 0.55595(19) 0.03944(16) 0.0535(6) Uani 1 1 d . .
F2 F 0.6779(2) 0.7201(2) -0.03619(14) 0.0466(5) Uani 1 1 d . .
F3 F 0.5553(2) 0.6509(2) 0.06814(16) 0.0491(5) Uani 1 1 d . .
C16 C 0.6831(3) 0.6674(3) 0.0513(2) 0.0336(7) Uani 1 1 d . .
C5 C 0.1416(5) 0.7684(5) -0.0238(3) 0.0654(13) Uani 1 1 d . .
H5A H 0.2039 0.7003 -0.0130 0.098 Uiso 1 1 calc R U
H5B H 0.0597 0.7416 -0.0632 0.098 Uiso 1 1 calc R U
H5C H 0.1190 0.7985 0.0388 0.098 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'
F F 0.0171 0.0103 '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 138.25(13) . .
C4 Zn1 N1 112.33(13) . .
O1 Zn1 N1 91.25(9) . .
C4 Zn1 O1 119.09(12) . 3_675
O1 Zn1 O1 80.87(9) . 3_675
N1 Zn1 O1 109.41(9) . 3_675
C4 Zn1 Zn1 143.69(10) . 3_675
O1 Zn1 Zn1 41.44(6) . 3_675
N1 Zn1 Zn1 103.70(7) . 3_675
O1 Zn1 Zn1 39.42(5) 3_675 3_675
C3 O1 Zn1 122.97(18) . .
C3 O1 Zn1 119.29(18) . 3_675
Zn1 O1 Zn1 99.13(9) . 3_675
C11 C10 C15 117.6(3) . .
C11 C10 C3 118.1(3) . .
C15 C10 C3 124.3(3) . .
N1 C1 C6 119.7(3) . .
N1 C1 C2 120.9(3) . .
C6 C1 C2 119.3(3) . .
C14 C15 C10 120.0(3) . .
C14 C15 C16 117.8(3) . .
C10 C15 C16 122.1(3) . .
C6 C7 C8 119.1(3) . .
N1 C9 C8 123.6(3) . .
O1 C3 C2 126.1(3) . .
O1 C3 C10 115.2(2) . .
C2 C3 C10 118.6(2) . .
C3 C2 C1 129.4(3) . .
C12 C11 C10 121.9(3) . .
C5 C4 Zn1 114.1(2) . .
C13 C12 C11 119.9(3) . .
C7 C6 C1 120.7(3) . .
C12 C13 C14 119.8(3) . .
C9 C8 C7 118.1(3) . .
C13 C14 C15 120.8(3) . .
C9 N1 C1 118.7(3) . .
C9 N1 Zn1 117.5(2) . .
C1 N1 Zn1 123.2(2) . .
F2 C16 F3 106.0(3) . .
F2 C16 F1 105.4(3) . .
F3 C16 F1 105.6(3) . .
F2 C16 C15 113.5(3) . .
F3 C16 C15 113.5(3) . .
F1 C16 C15 112.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 C4 1.964(3) .
Zn1 O1 2.006(2) .
Zn1 N1 2.083(2) .
Zn1 O1 2.091(2) 3_675
Zn1 Zn1 3.1188(7) 3_675
O1 C3 1.333(3) .
O1 Zn1 2.091(2) 3_675
C10 C11 1.395(4) .
C10 C15 1.404(4) .
C10 C3 1.489(4) .
C1 N1 1.357(4) .
C1 C6 1.397(4) .
C1 C2 1.449(4) .
C15 C14 1.390(4) .
C15 C16 1.499(4) .
C7 C6 1.368(5) .
C7 C8 1.389(5) .
C9 N1 1.348(4) .
C9 C8 1.367(5) .
C3 C2 1.351(4) .
C11 C12 1.381(4) .
C4 C5 1.512(5) .
C12 C13 1.371(6) .
C13 C14 1.382(5) .
F1 C16 1.345(4) .
F2 C16 1.341(4) .
F3 C16 1.342(4) .
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
C11 C10 C15 C14 -0.4(4) .
C3 C10 C15 C14 178.3(3) .
C11 C10 C15 C16 177.1(3) .
C3 C10 C15 C16 -4.3(4) .
Zn1 O1 C3 C2 -15.3(4) .
Zn1 O1 C3 C2 110.2(3) 3_675
Zn1 O1 C3 C10 167.99(19) .
Zn1 O1 C3 C10 -66.5(3) 3_675
C11 C10 C3 O1 127.6(3) .
C15 C10 C3 O1 -51.0(4) .
C11 C10 C3 C2 -49.4(4) .
C15 C10 C3 C2 132.0(3) .
O1 C3 C2 C1 -6.3(5) .
C10 C3 C2 C1 170.3(3) .
N1 C1 C2 C3 7.6(5) .
C6 C1 C2 C3 -170.1(3) .
C15 C10 C11 C12 0.1(5) .
C3 C10 C11 C12 -178.7(3) .
C10 C11 C12 C13 0.2(5) .
C8 C7 C6 C1 1.0(5) .
N1 C1 C6 C7 -1.6(5) .
C2 C1 C6 C7 176.1(3) .
C11 C12 C13 C14 -0.3(6) .
N1 C9 C8 C7 -1.7(5) .
C6 C7 C8 C9 0.6(5) .
C12 C13 C14 C15 0.0(6) .
C10 C15 C14 C13 0.3(5) .
C16 C15 C14 C13 -177.2(3) .
C8 C9 N1 C1 1.1(5) .
C8 C9 N1 Zn1 172.4(3) .
C6 C1 N1 C9 0.6(4) .
C2 C1 N1 C9 -177.1(3) .
C6 C1 N1 Zn1 -170.2(2) .
C2 C1 N1 Zn1 12.1(4) .
C14 C15 C16 F2 -99.4(3) .
C10 C15 C16 F2 83.1(4) .
C14 C15 C16 F3 139.4(3) .
C10 C15 C16 F3 -38.1(4) .
C14 C15 C16 F1 19.9(4) .
C10 C15 C16 F1 -157.6(3) .
