#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:36:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179148 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/09/4310967.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_4310967
loop_
_publ_author_name
'Eva Schön'
'Dietmar A. Plattner'
'Peter Chen'
_publ_section_title
;
 Defect-Induced Acceleration of a Solid-State Chemical Reaction in Zinc
 Alkoxide Single Crystals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3164
_journal_page_last               3169
_journal_paper_doi               10.1021/ic030341o
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C29 H36 N2 O2 Zn'
_chemical_formula_weight         509.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.39(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.10(2)
_cell_length_b                   14.89(2)
_cell_length_c                   11.94(2)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.56
_cell_measurement_theta_min      17.83
_cell_volume                     2668(7)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        MolEN
_computing_molecular_graphics    'Ortep, Pluto'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.688
_diffrn_measured_fraction_theta_max 0.688
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       ο/2π
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2876
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4850
_diffrn_reflns_theta_full        64.54
_diffrn_reflns_theta_max         64.54
_diffrn_reflns_theta_min         2.94
_diffrn_standards_interval_time  10000s
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.7085
_exptl_absorpt_correction_T_min  0.5555
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.802
_refine_diff_density_min         -2.618
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.595
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      3.929
_refine_ls_R_factor_all          0.2202
_refine_ls_R_factor_gt           0.1635
_refine_ls_shift/su_max          0.207
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3840
_refine_ls_wR_factor_ref         0.4626
_reflns_number_gt                3084
_reflns_number_total             4276
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            ic030341o_s_7.cif
_cod_data_source_block           XRD_7_2atoluene
_cod_database_code               4310967
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.21614(9) 0.37436(8) 0.19818(11) 0.0412(6) Uani 1 1 d . . .
O4 O 0.2899(5) 0.2762(5) 0.2515(6) 0.0524(19) Uani 1 1 d . . .
O5 O 0.1140(5) 0.3922(4) 0.2754(6) 0.0440(18) Uani 1 1 d . . .
N2 N 0.2712(6) 0.4953(6) 0.2397(8) 0.048(2) Uani 1 1 d . . .
N3 N 0.1803(5) 0.3251(5) 0.0431(7) 0.0393(19) Uani 1 1 d . . .
C6 C 0.2224(7) 0.5565(6) 0.2751(9) 0.048(3) Uani 1 1 d . . .
H6 H 0.2512 0.6122 0.2925 0.058 Uiso 1 1 calc R . .
C7 C 0.1320(7) 0.5531(7) 0.2920(9) 0.048(3) Uani 1 1 d . . .
C8 C 0.0905(9) 0.6352(8) 0.3151(12) 0.066(4) Uani 1 1 d . . .
H8 H 0.1246 0.6889 0.3166 0.079 Uiso 1 1 calc R . .
C9 C 0.0063(10) 0.6403(10) 0.3346(13) 0.078(4) Uani 1 1 d . . .
H9 H -0.0211 0.6971 0.3422 0.093 Uiso 1 1 calc R . .
C10 C -0.0420(9) 0.5612(11) 0.3438(11) 0.075(4) Uani 1 1 d . . .
H10 H -0.1009 0.5646 0.3645 0.091 Uiso 1 1 calc R . .
C11 C -0.0059(7) 0.4774(8) 0.3235(10) 0.053(3) Uani 1 1 d . . .
C12 C 0.0827(7) 0.4720(7) 0.2971(9) 0.045(2) Uani 1 1 d . . .
C13 C -0.0568(9) 0.3919(9) 0.3322(13) 0.074(4) Uani 1 1 d . . .
H13A H -0.0200 0.3489 0.3788 0.111 Uiso 1 1 calc R . .
H13B H -0.0722 0.3667 0.2567 0.111 Uiso 1 1 calc R . .
H13C H -0.1114 0.4042 0.3668 0.111 Uiso 1 1 calc R . .
C14 C 0.3657(7) 0.5123(8) 0.2391(9) 0.051(3) Uani 1 1 d . . .
H14 H 0.3772 0.5779 0.2517 0.062 Uiso 1 1 calc R . .
C15 C 0.4201(9) 0.4594(10) 0.3328(11) 0.070(4) Uani 1 1 d . . .
H15A H 0.4103 0.4847 0.4062 0.106 Uiso 1 1 calc R . .
H15B H 0.4835 0.4633 0.3227 0.106 Uiso 1 1 calc R . .
H15C H 0.4013 0.3964 0.3294 0.106 Uiso 1 1 calc R . .
C16 C 0.3917(9) 0.4865(10) 0.1235(11) 0.074(4) Uani 1 1 d . . .
H16A H 0.4527 0.5065 0.1170 0.111 Uiso 1 1 calc R . .
H16B H 0.3508 0.5153 0.0647 0.111 Uiso 1 1 calc R . .
H16C H 0.3881 0.4211 0.1144 0.111 Uiso 1 1 calc R . .
C17 C 0.1992(6) 0.2441(6) 0.0179(8) 0.039(2) Uani 1 1 d . . .
H17 H 0.1782 0.2239 -0.0558 0.046 Uiso 1 1 calc R . .
C18 C 0.2501(7) 0.1799(6) 0.0927(10) 0.043(2) Uani 1 1 d . . .
C19 C 0.2560(8) 0.0928(7) 0.0467(11) 0.054(3) Uani 1 1 d . . .
H19 H 0.2296 0.0807 -0.0278 0.064 Uiso 1 1 calc R . .
C20 C 0.2993(9) 0.0262(7) 0.1089(15) 0.072(4) Uani 1 1 d . . .
H20 H 0.2988 -0.0332 0.0798 0.087 Uiso 1 1 calc R . .
C21 C 0.3433(9) 0.0438(8) 0.2127(13) 0.065(4) Uani 1 1 d . . .
H21 H 0.3770 -0.0028 0.2516 0.078 Uiso 1 1 calc R . .
C22 C 0.3404(8) 0.1279(7) 0.2633(11) 0.055(3) Uani 1 1 d . . .
C23 C 0.2927(6) 0.1984(6) 0.2027(9) 0.041(2) Uani 1 1 d . . .
C24 C 0.3892(9) 0.1517(10) 0.3735(12) 0.075(4) Uani 1 1 d . . .
H24A H 0.4160 0.0975 0.4095 0.112 Uiso 1 1 calc R . .
H24B H 0.3478 0.1783 0.4218 0.112 Uiso 1 1 calc R . .
H24C H 0.4362 0.1951 0.3622 0.112 Uiso 1 1 calc R . .
C25 C 0.1241(7) 0.3761(7) -0.0451(10) 0.048(3) Uani 1 1 d . . .
H25 H 0.1276 0.3458 -0.1192 0.058 Uiso 1 1 calc R . .
C26 C 0.1588(8) 0.4700(8) -0.0527(12) 0.068(4) Uani 1 1 d . . .
H26A H 0.1546 0.5012 0.0188 0.101 Uiso 1 1 calc R . .
H26B H 0.1233 0.5020 -0.1138 0.101 Uiso 1 1 calc R . .
H26C H 0.2212 0.4680 -0.0681 0.101 Uiso 1 1 calc R . .
C27 C 0.0289(8) 0.3743(8) -0.0200(12) 0.062(3) Uani 1 1 d . . .
H27A H 0.0118 0.3124 -0.0044 0.093 Uiso 1 1 calc R . .
H27B H -0.0097 0.3973 -0.0851 0.093 Uiso 1 1 calc R . .
H27C H 0.0224 0.4119 0.0460 0.093 Uiso 1 1 calc R . .
C28 C 0.2453(15) 0.7032(16) -0.016(3) 0.170(14) Uani 1 1 d . . .
H28 H 0.1888 0.6848 0.0040 0.204 Uiso 1 1 calc R . .
C29 C 0.2973(18) 0.7531(14) 0.028(2) 0.150(11) Uani 1 1 d . . .
H29 H 0.2777 0.7757 0.0957 0.180 Uiso 1 1 calc R . .
C30 C 0.3818(13) 0.7906(11) 0.0112(15) 0.091(5) Uani 1 1 d . . .
H30 H 0.4077 0.8352 0.0614 0.109 Uiso 1 1 calc R . .
C31 C 0.424(3) 0.763(2) -0.074(2) 0.180(16) Uani 1 1 d . . .
C32 C 0.377(2) 0.6942(14) -0.163(2) 0.134(10) Uani 1 1 d . . .
H32 H 0.3994 0.6725 -0.2298 0.161 Uiso 1 1 calc R . .
C33 C 0.301(3) 0.6735(17) -0.1247(19) 0.158(14) Uani 1 1 d . . .
H33 H 0.2688 0.6301 -0.1712 0.189 Uiso 1 1 calc R . .
C34 C 0.4946(15) 0.7777(17) -0.112(2) 0.159(12) Uani 1 1 d . . .
H34A H 0.5019 0.8425 -0.1227 0.238 Uiso 1 1 calc R . .
H34B H 0.4944 0.7472 -0.1852 0.238 Uiso 1 1 calc R . .
H34C H 0.5441 0.7549 -0.0600 0.238 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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
O5 Zn1 O4 114.9(3) . . ?
O5 Zn1 N3 110.4(3) . . ?
O4 Zn1 N3 96.7(3) . . ?
O5 Zn1 N2 95.2(3) . . ?
O4 Zn1 N2 113.1(4) . . ?
N3 Zn1 N2 127.7(3) . . ?
C23 O4 Zn1 125.5(7) . . ?
C12 O5 Zn1 123.5(7) . . ?
C6 N2 C14 118.9(9) . . ?
C6 N2 Zn1 118.8(8) . . ?
C14 N2 Zn1 122.1(7) . . ?
C17 N3 C25 116.0(9) . . ?
C17 N3 Zn1 121.0(7) . . ?
C25 N3 Zn1 122.7(6) . . ?
N2 C6 C7 129.1(10) . . ?
C6 C7 C8 117.1(11) . . ?
C6 C7 C12 124.0(9) . . ?
C8 C7 C12 118.7(11) . . ?
C9 C8 C7 122.7(13) . . ?
C8 C9 C10 119.2(11) . . ?
C11 C10 C9 121.6(12) . . ?
C10 C11 C12 119.3(12) . . ?
C10 C11 C13 122.4(12) . . ?
C12 C11 C13 118.3(10) . . ?
O5 C12 C11 117.9(10) . . ?
O5 C12 C7 123.8(10) . . ?
C11 C12 C7 118.3(10) . . ?
N2 C14 C16 108.2(9) . . ?
N2 C14 C15 110.8(9) . . ?
C16 C14 C15 111.1(11) . . ?
N3 C17 C18 125.8(10) . . ?
C19 C18 C23 119.6(9) . . ?
C19 C18 C17 114.4(10) . . ?
C23 C18 C17 126.0(9) . . ?
C20 C19 C18 120.1(12) . . ?
C19 C20 C21 120.8(11) . . ?
C20 C21 C22 122.0(11) . . ?
C21 C22 C23 118.8(13) . . ?
C21 C22 C24 124.4(11) . . ?
C23 C22 C24 116.7(11) . . ?
O4 C23 C22 118.0(10) . . ?
O4 C23 C18 123.5(9) . . ?
C22 C23 C18 118.5(10) . . ?
N3 C25 C26 110.1(9) . . ?
N3 C25 C27 109.5(10) . . ?
C26 C25 C27 112.2(9) . . ?
C29 C28 C33 98(3) . . ?
C28 C29 C30 139(3) . . ?
C31 C30 C29 120(3) . . ?
C34 C31 C30 139(4) . . ?
C34 C31 C32 102(3) . . ?
C30 C31 C32 119(3) . . ?
C33 C32 C31 105(3) . . ?
C32 C33 C28 137(3) . . ?
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 O5 1.901(7) . ?
Zn1 O4 1.904(7) . ?
Zn1 N3 2.009(9) . ?
Zn1 N2 2.022(9) . ?
O4 C23 1.301(12) . ?
O5 C12 1.316(12) . ?
N2 C6 1.273(13) . ?
N2 C14 1.451(14) . ?
N3 C17 1.282(12) . ?
N3 C25 1.485(13) . ?
C6 C7 1.403(15) . ?
C7 C8 1.415(14) . ?
C7 C12 1.423(16) . ?
C8 C9 1.32(2) . ?
C9 C10 1.40(2) . ?
C10 C11 1.393(18) . ?
C11 C12 1.410(16) . ?
C11 C13 1.497(17) . ?
C14 C16 1.526(17) . ?
C14 C15 1.529(17) . ?
C17 C18 1.467(14) . ?
C18 C19 1.415(14) . ?
C18 C23 1.423(16) . ?
C19 C20 1.362(18) . ?
C20 C21 1.36(2) . ?
C21 C22 1.394(17) . ?
C22 C23 1.424(14) . ?
C22 C24 1.478(19) . ?
C25 C26 1.499(15) . ?
C25 C27 1.502(17) . ?
C28 C29 1.16(3) . ?
C28 C33 1.69(4) . ?
C29 C30 1.43(3) . ?
C30 C31 1.33(3) . ?
C31 C34 1.22(4) . ?
C31 C32 1.59(4) . ?
C32 C33 1.33(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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Zn1 O4 C23 103.0(8) . . . . ?
N3 Zn1 O4 C23 -13.2(9) . . . . ?
N2 Zn1 O4 C23 -149.2(8) . . . . ?
O4 Zn1 O5 C12 143.1(8) . . . . ?
N3 Zn1 O5 C12 -108.9(8) . . . . ?
N2 Zn1 O5 C12 24.7(9) . . . . ?
O5 Zn1 N2 C6 -16.9(9) . . . . ?
O4 Zn1 N2 C6 -136.8(8) . . . . ?
N3 Zn1 N2 C6 103.9(9) . . . . ?
O5 Zn1 N2 C14 158.0(8) . . . . ?
O4 Zn1 N2 C14 38.1(9) . . . . ?
N3 Zn1 N2 C14 -81.2(9) . . . . ?
O5 Zn1 N3 C17 -110.3(7) . . . . ?
O4 Zn1 N3 C17 9.4(8) . . . . ?
N2 Zn1 N3 C17 135.6(7) . . . . ?
O5 Zn1 N3 C25 63.9(8) . . . . ?
O4 Zn1 N3 C25 -176.4(7) . . . . ?
N2 Zn1 N3 C25 -50.3(9) . . . . ?
C14 N2 C6 C7 -174.3(11) . . . . ?
Zn1 N2 C6 C7 0.8(16) . . . . ?
N2 C6 C7 C8 -170.2(12) . . . . ?
N2 C6 C7 C12 15.6(19) . . . . ?
C6 C7 C8 C9 -178.7(13) . . . . ?
C12 C7 C8 C9 -4.1(19) . . . . ?
C7 C8 C9 C10 6(2) . . . . ?
C8 C9 C10 C11 -6(2) . . . . ?
C9 C10 C11 C12 2(2) . . . . ?
C9 C10 C11 C13 -179.6(13) . . . . ?
Zn1 O5 C12 C11 161.5(8) . . . . ?
Zn1 O5 C12 C7 -16.5(14) . . . . ?
C10 C11 C12 O5 -178.2(11) . . . . ?
C13 C11 C12 O5 3.7(16) . . . . ?
C10 C11 C12 C7 -0.1(17) . . . . ?
C13 C11 C12 C7 -178.2(11) . . . . ?
C6 C7 C12 O5 -7.1(17) . . . . ?
C8 C7 C12 O5 178.8(10) . . . . ?
C6 C7 C12 C11 175.0(10) . . . . ?
C8 C7 C12 C11 0.8(16) . . . . ?
C6 N2 C14 C16 -131.0(11) . . . . ?
Zn1 N2 C14 C16 54.1(12) . . . . ?
C6 N2 C14 C15 106.9(12) . . . . ?
Zn1 N2 C14 C15 -68.1(11) . . . . ?
C25 N3 C17 C18 -177.2(9) . . . . ?
Zn1 N3 C17 C18 -2.7(13) . . . . ?
N3 C17 C18 C19 175.7(9) . . . . ?
N3 C17 C18 C23 -4.9(16) . . . . ?
C23 C18 C19 C20 2.4(16) . . . . ?
C17 C18 C19 C20 -178.1(10) . . . . ?
C18 C19 C20 C21 -5.0(18) . . . . ?
C19 C20 C21 C22 5.1(19) . . . . ?
C20 C21 C22 C23 -2.4(18) . . . . ?
C20 C21 C22 C24 -177.7(13) . . . . ?
Zn1 O4 C23 C22 -169.7(7) . . . . ?
Zn1 O4 C23 C18 9.7(14) . . . . ?
C21 C22 C23 O4 179.3(10) . . . . ?
C24 C22 C23 O4 -5.0(15) . . . . ?
C21 C22 C23 C18 -0.1(15) . . . . ?
C24 C22 C23 C18 175.5(10) . . . . ?
C19 C18 C23 O4 -179.3(9) . . . . ?
C17 C18 C23 O4 1.3(16) . . . . ?
C19 C18 C23 C22 0.1(15) . . . . ?
C17 C18 C23 C22 -179.3(10) . . . . ?
C17 N3 C25 C26 -137.7(10) . . . . ?
Zn1 N3 C25 C26 47.9(12) . . . . ?
C17 N3 C25 C27 98.5(11) . . . . ?
Zn1 N3 C25 C27 -75.9(10) . . . . ?
C33 C28 C29 C30 2(4) . . . . ?
C28 C29 C30 C31 -5(4) . . . . ?
C29 C30 C31 C34 -178(3) . . . . ?
C29 C30 C31 C32 5(3) . . . . ?
C34 C31 C32 C33 178(2) . . . . ?
C30 C31 C32 C33 -4(3) . . . . ?
C31 C32 C33 C28 2(4) . . . . ?
C29 C28 C33 C32 -2(4) . . . . ?
