#------------------------------------------------------------------------------
#$Date: 2016-03-26 23:00:42 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180526 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/95/7219579.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_7219579
loop_
_publ_author_name
'Rojas, Rene S.'
'Trofymchuk, Oleksandra S.'
'Daniliuc, Constantin Gabriel'
'Kehr, Gerald'
'Erker, G.'
_publ_section_title
;
 Synthesis and Structures of N-Arylcyano-β-diketiminate Zinc Complexes
 and Adducts, their Application in Ring‐Opening Polymerization of
 L-lactide
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA16670A
_journal_year                    2015
_chemical_formula_sum            'C48 H58 N6 O2 Zn2'
_chemical_formula_weight         881.74
_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
_audit_update_record
;
2015-01-27 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                101.950(2)
_cell_angle_beta                 104.633(2)
_cell_angle_gamma                104.7120(10)
_cell_formula_units_Z            1
_cell_length_a                   9.7845(3)
_cell_length_b                   10.2261(4)
_cell_length_c                   12.4486(4)
_cell_measurement_reflns_used    4376
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     1115.63(7)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14401
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    1.120
_exptl_absorpt_correction_T_max  0.9257
_exptl_absorpt_correction_T_min  0.8500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0404P)²+0.4287P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                4207
_reflns_number_total             4478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra16670a2.cif
_cod_data_source_block           erk7487
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7219579
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 0.65008(2) 0.60964(2) 0.532559(16) 0.03904(9) Uani 1 1 d .
O1 O 0.56211(16) 0.41763(14) 0.54076(12) 0.0480(3) Uani 1 1 d D
H01 H 0.599(3) 0.367(2) 0.574(2) 0.058 Uiso 1 1 d D
N1 N 0.78747(18) 0.62703(18) 0.43803(13) 0.0453(4) Uani 1 1 d .
N2 N 0.77712(17) 0.77555(16) 0.66812(12) 0.0387(3) Uani 1 1 d .
C1 C 0.9153(2) 0.7337(2) 0.47343(17) 0.0475(4) Uani 1 1 d .
C2 C 0.9679(2) 0.8386(2) 0.57945(17) 0.0486(4) Uani 1 1 d .
H2 H 1.0590 0.9080 0.5924 0.058 Uiso 1 1 calc R
C3 C 0.9074(2) 0.8573(2) 0.66925(16) 0.0430(4) Uani 1 1 d .
C4 C 1.0156(3) 0.7429(3) 0.3982(2) 0.0632(6) Uani 1 1 d .
H4A H 1.0512 0.6623 0.3911 0.095 Uiso 1 1 calc R
H4B H 1.1000 0.8293 0.4336 0.095 Uiso 1 1 calc R
H4C H 0.9597 0.7431 0.3219 0.095 Uiso 1 1 calc R
C5 C 1.0029(2) 0.9796(2) 0.77604(18) 0.0536(5) Uani 1 1 d .
H5A H 0.9472 1.0434 0.7916 0.080 Uiso 1 1 calc R
H5B H 1.0927 1.0298 0.7629 0.080 Uiso 1 1 calc R
H5C H 1.0299 0.9439 0.8420 0.080 Uiso 1 1 calc R
C11 C 0.7544(2) 0.5213(2) 0.33190(17) 0.0469(4) Uani 1 1 d .
C12 C 0.6812(2) 0.5358(2) 0.22623(17) 0.0518(5) Uani 1 1 d .
C13 C 0.6508(3) 0.4316(3) 0.1225(2) 0.0671(7) Uani 1 1 d .
H13 H 0.6010 0.4422 0.0512 0.080 Uiso 1 1 calc R
C14 C 0.6934(3) 0.3150(3) 0.1249(2) 0.0763(8) Uani 1 1 d .
H14 H 0.6739 0.2456 0.0554 0.092 Uiso 1 1 calc R
C15 C 0.7650(4) 0.2989(3) 0.2293(3) 0.0776(8) Uani 1 1 d .
H15 H 0.7941 0.2184 0.2307 0.093 Uiso 1 1 calc R
C16 C 0.7945(3) 0.4012(3) 0.3325(2) 0.0639(6) Uani 1 1 d .
H16 H 0.8421 0.3885 0.4034 0.077 Uiso 1 1 calc R
C17 C 0.6445(3) 0.6610(3) 0.2207(2) 0.0652(6) Uani 1 1 d .
N17 N 0.6178(4) 0.7617(3) 0.2106(3) 0.0950(9) Uani 1 1 d .
C21 C 0.7318(2) 0.81382(19) 0.76876(15) 0.0417(4) Uani 1 1 d .
C22 C 0.7740(2) 0.7598(2) 0.86229(16) 0.0457(4) Uani 1 1 d .
C23 C 0.7323(2) 0.8023(3) 0.95960(17) 0.0544(5) Uani 1 1 d .
H23 H 0.7580 0.7660 1.0225 0.065 Uiso 1 1 calc R
C24 C 0.6536(3) 0.8971(3) 0.96499(19) 0.0619(6) Uani 1 1 d .
H24 H 0.6286 0.9266 1.0320 0.074 Uiso 1 1 calc R
C25 C 0.6125(3) 0.9476(3) 0.8729(2) 0.0588(6) Uani 1 1 d .
H25 H 0.5579 1.0110 0.8773 0.071 Uiso 1 1 calc R
C26 C 0.6490(2) 0.9078(2) 0.77212(17) 0.0479(4) Uani 1 1 d .
C27 C 0.8648(3) 0.6598(2) 0.86145(18) 0.0535(5) Uani 1 1 d .
H27 H 0.9054 0.6611 0.7963 0.064 Uiso 1 1 calc R
C28 C 0.7667(4) 0.5086(3) 0.8406(3) 0.0841(9) Uani 1 1 d .
H28A H 0.7324 0.5026 0.9066 0.126 Uiso 1 1 calc R
H28B H 0.8240 0.4449 0.8307 0.126 Uiso 1 1 calc R
H28C H 0.6813 0.4822 0.7712 0.126 Uiso 1 1 calc R
C29 C 0.9973(3) 0.7042(3) 0.9737(2) 0.0710(7) Uani 1 1 d .
H29A H 1.0562 0.8019 0.9888 0.107 Uiso 1 1 calc R
H29B H 1.0589 0.6444 0.9652 0.107 Uiso 1 1 calc R
H29C H 0.9603 0.6942 1.0378 0.107 Uiso 1 1 calc R
C30 C 0.6030(3) 0.9699(2) 0.6737(2) 0.0553(5) Uani 1 1 d .
H30 H 0.6404 0.9318 0.6113 0.066 Uiso 1 1 calc R
C31 C 0.4326(3) 0.9266(3) 0.6236(2) 0.0701(7) Uani 1 1 d .
H31A H 0.3908 0.8244 0.5957 0.105 Uiso 1 1 calc R
H31B H 0.4060 0.9659 0.5599 0.105 Uiso 1 1 calc R
H31C H 0.3932 0.9620 0.6836 0.105 Uiso 1 1 calc R
C32 C 0.6708(3) 1.1307(3) 0.7121(3) 0.0702(7) Uani 1 1 d .
H32A H 0.6337 1.1706 0.7720 0.105 Uiso 1 1 calc R
H32B H 0.6433 1.1664 0.6462 0.105 Uiso 1 1 calc R
H32C H 0.7787 1.1572 0.7425 0.105 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'
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
O1 Zn1 O1 80.56(6) 2_666 .
O1 Zn1 N2 121.14(6) 2_666 .
O1 Zn1 N2 125.14(6) . .
O1 Zn1 N1 119.27(6) 2_666 .
O1 Zn1 N1 115.46(7) . .
N2 Zn1 N1 97.24(6) . .
O1 Zn1 Zn1 40.31(4) 2_666 2_666
O1 Zn1 Zn1 40.24(4) . 2_666
N2 Zn1 Zn1 135.74(5) . 2_666
N1 Zn1 Zn1 127.02(5) . 2_666
Zn1 O1 Zn1 99.44(6) 2_666 .
Zn1 O1 H01 128.1(18) 2_666 .
Zn1 O1 H01 131.7(18) . .
C1 N1 C11 117.66(16) . .
C1 N1 Zn1 121.70(13) . .
C11 N1 Zn1 120.59(13) . .
C3 N2 C21 117.02(15) . .
C3 N2 Zn1 121.17(12) . .
C21 N2 Zn1 121.80(12) . .
N1 C1 C2 124.05(18) . .
N1 C1 C4 119.79(18) . .
C2 C1 C4 116.13(19) . .
C3 C2 C1 130.56(19) . .
C3 C2 H2 114.7 . .
C1 C2 H2 114.7 . .
N2 C3 C2 125.16(17) . .
N2 C3 C5 119.35(17) . .
C2 C3 C5 115.47(18) . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C16 C11 C12 118.5(2) . .
C16 C11 N1 120.3(2) . .
C12 C11 N1 121.17(19) . .
C11 C12 C13 120.5(2) . .
C11 C12 C17 120.5(2) . .
C13 C12 C17 118.8(2) . .
C14 C13 C12 120.0(2) . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C13 C14 C15 120.0(2) . .
C13 C14 H14 120.0 . .
C15 C14 H14 120.0 . .
C14 C15 C16 120.4(3) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C11 C16 C15 120.6(2) . .
C11 C16 H16 119.7 . .
C15 C16 H16 119.7 . .
N17 C17 C12 176.0(3) . .
C22 C21 C26 121.24(17) . .
C22 C21 N2 119.74(17) . .
C26 C21 N2 119.01(17) . .
C23 C22 C21 118.3(2) . .
C23 C22 C27 119.44(19) . .
C21 C22 C27 122.27(17) . .
C24 C23 C22 121.0(2) . .
C24 C23 H23 119.5 . .
C22 C23 H23 119.5 . .
C25 C24 C23 119.90(19) . .
C25 C24 H24 120.1 . .
C23 C24 H24 120.1 . .
C24 C25 C26 121.9(2) . .
C24 C25 H25 119.0 . .
C26 C25 H25 119.0 . .
C25 C26 C21 117.6(2) . .
C25 C26 C30 119.4(2) . .
C21 C26 C30 122.91(18) . .
C22 C27 C28 110.9(2) . .
C22 C27 C29 112.55(18) . .
C28 C27 C29 109.8(2) . .
C22 C27 H27 107.8 . .
C28 C27 H27 107.8 . .
C29 C27 H27 107.8 . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C26 C30 C32 111.7(2) . .
C26 C30 C31 111.1(2) . .
C32 C30 C31 110.0(2) . .
C26 C30 H30 108.0 . .
C32 C30 H30 108.0 . .
C31 C30 H30 108.0 . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C30 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.9658(14) 2_666
Zn1 O1 1.9687(14) .
Zn1 N2 1.9886(14) .
Zn1 N1 1.9970(16) .
Zn1 Zn1 3.0017(4) 2_666
O1 Zn1 1.9658(14) 2_666
O1 H01 0.822(16) .
N1 C1 1.333(3) .
N1 C11 1.426(2) .
N2 C3 1.330(2) .
N2 C21 1.444(2) .
C1 C2 1.395(3) .
C1 C4 1.517(3) .
C2 C3 1.393(3) .
C2 H2 0.9400 .
C3 C5 1.515(3) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C4 H4C 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C5 H5C 0.9700 .
C11 C16 1.382(3) .
C11 C12 1.387(3) .
C12 C13 1.402(3) .
C12 C17 1.425(4) .
C13 C14 1.364(4) .
C13 H13 0.9400 .
C14 C15 1.375(4) .
C14 H14 0.9400 .
C15 C16 1.390(4) .
C15 H15 0.9400 .
C16 H16 0.9400 .
C17 N17 1.148(4) .
C21 C22 1.403(3) .
C21 C26 1.406(3) .
C22 C23 1.394(3) .
C22 C27 1.516(3) .
C23 C24 1.384(3) .
C23 H23 0.9400 .
C24 C25 1.364(4) .
C24 H24 0.9400 .
C25 C26 1.399(3) .
C25 H25 0.9400 .
C26 C30 1.515(3) .
C27 C28 1.528(4) .
C27 C29 1.536(3) .
C27 H27 0.9900 .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C28 H28C 0.9700 .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
C29 H29C 0.9700 .
C30 C32 1.527(3) .
C30 C31 1.533(4) .
C30 H30 0.9900 .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C31 H31C 0.9700 .
C32 H32A 0.9700 .
C32 H32B 0.9700 .
C32 H32C 0.9700 .
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
O1 Zn1 O1 Zn1 0.0 2_666 2_666
N2 Zn1 O1 Zn1 121.60(7) . 2_666
N1 Zn1 O1 Zn1 -118.02(7) . 2_666
O1 Zn1 N1 C1 128.62(16) 2_666 .
O1 Zn1 N1 C1 -138.03(16) . .
N2 Zn1 N1 C1 -3.36(18) . .
Zn1 Zn1 N1 C1 176.39(14) 2_666 .
O1 Zn1 N1 C11 -54.08(17) 2_666 .
O1 Zn1 N1 C11 39.27(17) . .
N2 Zn1 N1 C11 173.94(15) . .
Zn1 Zn1 N1 C11 -6.32(18) 2_666 .
O1 Zn1 N2 C3 -128.85(14) 2_666 .
O1 Zn1 N2 C3 130.15(14) . .
N1 Zn1 N2 C3 1.89(16) . .
Zn1 Zn1 N2 C3 -177.82(12) 2_666 .
O1 Zn1 N2 C21 50.35(16) 2_666 .
O1 Zn1 N2 C21 -50.66(16) . .
N1 Zn1 N2 C21 -178.92(14) . .
Zn1 Zn1 N2 C21 1.38(17) 2_666 .
C11 N1 C1 C2 -174.8(2) . .
Zn1 N1 C1 C2 2.6(3) . .
C11 N1 C1 C4 3.0(3) . .
Zn1 N1 C1 C4 -179.61(16) . .
N1 C1 C2 C3 0.8(4) . .
C4 C1 C2 C3 -177.1(2) . .
C21 N2 C3 C2 -178.73(19) . .
Zn1 N2 C3 C2 0.5(3) . .
C21 N2 C3 C5 2.9(3) . .
Zn1 N2 C3 C5 -177.91(14) . .
C1 C2 C3 N2 -2.6(4) . .
C1 C2 C3 C5 175.9(2) . .
C1 N1 C11 C16 92.8(3) . .
Zn1 N1 C11 C16 -84.6(2) . .
C1 N1 C11 C12 -87.5(3) . .
Zn1 N1 C11 C12 95.1(2) . .
C16 C11 C12 C13 -1.0(3) . .
N1 C11 C12 C13 179.4(2) . .
C16 C11 C12 C17 -176.8(2) . .
N1 C11 C12 C17 3.6(3) . .
C11 C12 C13 C14 -0.1(4) . .
C17 C12 C13 C14 175.8(2) . .
C12 C13 C14 C15 0.6(4) . .
C13 C14 C15 C16 -0.1(4) . .
C12 C11 C16 C15 1.5(4) . .
N1 C11 C16 C15 -178.8(2) . .
C14 C15 C16 C11 -1.0(4) . .
C11 C12 C17 N17 137(5) . .
C13 C12 C17 N17 -39(5) . .
C3 N2 C21 C22 -89.4(2) . .
Zn1 N2 C21 C22 91.41(19) . .
C3 N2 C21 C26 89.0(2) . .
Zn1 N2 C21 C26 -90.19(19) . .
C26 C21 C22 C23 -0.3(3) . .
N2 C21 C22 C23 178.07(17) . .
C26 C21 C22 C27 -179.24(19) . .
N2 C21 C22 C27 -0.9(3) . .
C21 C22 C23 C24 -1.1(3) . .
C27 C22 C23 C24 177.9(2) . .
C22 C23 C24 C25 1.7(4) . .
C23 C24 C25 C26 -0.8(4) . .
C24 C25 C26 C21 -0.6(3) . .
C24 C25 C26 C30 -178.7(2) . .
C22 C21 C26 C25 1.1(3) . .
N2 C21 C26 C25 -177.26(18) . .
C22 C21 C26 C30 179.19(19) . .
N2 C21 C26 C30 0.8(3) . .
C23 C22 C27 C28 76.5(3) . .
C21 C22 C27 C28 -104.6(2) . .
C23 C22 C27 C29 -46.9(3) . .
C21 C22 C27 C29 132.0(2) . .
C25 C26 C30 C32 60.0(3) . .
C21 C26 C30 C32 -118.1(2) . .
C25 C26 C30 C31 -63.3(3) . .
C21 C26 C30 C31 118.7(2) . .
