#------------------------------------------------------------------------------
#$Date: 2017-09-13 04:49:39 +0300 (Wed, 13 Sep 2017) $
#$Revision: 200804 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/06/7120635.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_7120635
loop_
_publ_author_name
'Wróbel, Zbigniew'
'Pietrzak, Tomasz'
'Justyniak, Iwona'
'Lewinski, Janusz'
_publ_section_title
;
 Oxygenation of RZn(N,O)-type complexes as an efficient route to zinc
 alkoxides not accessible via classical alcoholysis path
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC05818G
_journal_year                    2017
_chemical_formula_sum            'C32 H42 N4 O9 Zn4'
_chemical_formula_weight         888.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-06-11 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.1610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0060(4)
_cell_length_b                   11.4160(2)
_cell_length_c                   18.1170(4)
_cell_measurement_reflns_used    4452
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3721.42(13)
_computing_cell_refinement       'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction        'Denzo & Scalepak (Otwinowski, Minor, 1997)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'area detector ω scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8133
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.113
_exptl_absorpt_coefficient_mu    2.602
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepak (Otwinowski, Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       plate
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0156P)²+15.9115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3632
_reflns_number_total             4264
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc05818g2.cif
_cod_data_source_block           shelx_comp3
_cod_database_code               7120635
_shelx_shelxl_version_number     2016/6
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_refinement_flags_occupancy
C1 C 0.39407(17) 0.4106(3) 0.13719(17) 0.0261(6) Uani 1 1 d . . .
C2 C 0.4487(2) 0.4546(3) 0.0813(2) 0.0448(9) Uani 1 1 d . . .
H2A H 0.448572 0.401295 0.038854 0.067 Uiso 1 1 calc R U .
H2B H 0.498783 0.457609 0.104429 0.067 Uiso 1 1 calc R U .
H2C H 0.434043 0.533170 0.064564 0.067 Uiso 1 1 calc R U .
C3 C 0.3917(2) 0.4979(3) 0.2015(2) 0.0434(9) Uani 1 1 d . . .
H3A H 0.376928 0.575165 0.182470 0.065 Uiso 1 1 calc R U .
H3B H 0.441099 0.503228 0.225937 0.065 Uiso 1 1 calc R U .
H3C H 0.355722 0.471119 0.237000 0.065 Uiso 1 1 calc R U .
C4 C 0.3165(2) 0.4058(3) 0.1011(3) 0.0569(12) Uani 1 1 d . . .
H4A H 0.301532 0.484470 0.084838 0.085 Uiso 1 1 calc R U .
H4B H 0.281342 0.376658 0.136859 0.085 Uiso 1 1 calc R U .
H4C H 0.316489 0.353092 0.058403 0.085 Uiso 1 1 calc R U .
C5 C 0.57005(17) -0.1588(3) 0.18943(16) 0.0245(6) Uani 1 1 d . . .
H5 H 0.610847 -0.171187 0.223304 0.029 Uiso 1 1 calc R U .
C6 C 0.52738(18) -0.2479(3) 0.15612(17) 0.0287(7) Uani 1 1 d . . .
H6 H 0.533707 -0.329834 0.163163 0.034 Uiso 1 1 calc R U .
C7 C 0.47382(17) -0.1933(3) 0.11061(16) 0.0256(6) Uani 1 1 d . . .
H7 H 0.436425 -0.230483 0.080540 0.031 Uiso 1 1 calc R U .
C8 C 0.48597(16) -0.0732(3) 0.11795(15) 0.0207(6) Uani 1 1 d . . .
C9 C 0.45129(15) 0.0255(3) 0.08421(14) 0.0195(6) Uani 1 1 d . . .
C10 C 0.36455(18) 0.0995(3) -0.00533(17) 0.0336(8) Uani 1 1 d . . .
H10A H 0.338533 0.150040 0.028995 0.050 Uiso 1 1 calc R U .
H10B H 0.329214 0.070705 -0.043590 0.050 Uiso 1 1 calc R U .
H10C H 0.403828 0.144436 -0.028431 0.050 Uiso 1 1 calc R U .
C11 C 0.65420(18) 0.2667(3) 0.08139(16) 0.0301(7) Uani 1 1 d . . .
H11 H 0.617958 0.271974 0.042041 0.036 Uiso 1 1 calc R U .
C12 C 0.72530(19) 0.3152(3) 0.08028(17) 0.0318(7) Uani 1 1 d . . .
H12 H 0.745322 0.359087 0.041142 0.038 Uiso 1 1 calc R U .
C13 C 0.76120(17) 0.2874(3) 0.14699(17) 0.0265(7) Uani 1 1 d . . .
H13 H 0.810579 0.307545 0.162405 0.032 Uiso 1 1 calc R U .
C14 C 0.71008(15) 0.2239(3) 0.18692(16) 0.0215(6) Uani 1 1 d . . .
C15 C 0.71298(15) 0.1736(2) 0.25850(16) 0.0199(6) Uani 1 1 d . . .
C16 C 0.78635(18) 0.1212(3) 0.36549(18) 0.0341(8) Uani 1 1 d . . .
H16A H 0.763969 0.171535 0.402427 0.051 Uiso 1 1 calc R U .
H16B H 0.839078 0.109310 0.378770 0.051 Uiso 1 1 calc R U .
H16C H 0.760838 0.045393 0.363902 0.051 Uiso 1 1 calc R U .
O1 O 0.500000 0.1943(2) 0.250000 0.0175(5) Uani 1 2 d S T P
O2 O 0.47065(11) 0.12896(17) 0.09833(10) 0.0206(4) Uani 1 1 d . . .
O3 O 0.39711(12) 0.0014(2) 0.03456(11) 0.0282(5) Uani 1 1 d . . .
O4 O 0.65698(11) 0.12945(17) 0.28756(11) 0.0223(4) Uani 1 1 d . . .
O5 O 0.77924(11) 0.17645(19) 0.29379(11) 0.0256(5) Uani 1 1 d . . .
N1 N 0.54536(13) -0.0531(2) 0.16690(12) 0.0190(5) Uani 1 1 d . . .
N2 N 0.64397(13) 0.2112(2) 0.14590(13) 0.0223(5) Uani 1 1 d . . .
Zn1 Zn 0.43028(2) 0.25898(3) 0.17703(2) 0.01986(9) Uani 1 1 d . . .
Zn2 Zn 0.56836(2) 0.10994(3) 0.18604(2) 0.01922(9) 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'
N N 0.0061 0.0033 '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 C1 C2 109.4(3) . .
C4 C1 C3 107.4(3) . .
C2 C1 C3 109.1(3) . .
C4 C1 Zn1 114.2(2) . .
C2 C1 Zn1 108.6(2) . .
C3 C1 Zn1 108.1(2) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
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 . .
N1 C5 C6 110.6(3) . .
N1 C5 H5 124.7 . .
C6 C5 H5 124.7 . .
C7 C6 C5 106.7(3) . .
C7 C6 H6 126.7 . .
C5 C6 H6 126.7 . .
C6 C7 C8 106.3(3) . .
C6 C7 H7 126.8 . .
C8 C7 H7 126.8 . .
N1 C8 C7 109.8(3) . .
N1 C8 C9 117.5(3) . .
C7 C8 C9 132.6(3) . .
O2 C9 O3 121.6(3) . .
O2 C9 C8 123.1(2) . .
O3 C9 C8 115.3(3) . .
O3 C10 H10A 109.5 . .
O3 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O3 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N2 C11 C12 110.7(3) . .
N2 C11 H11 124.6 . .
C12 C11 H11 124.6 . .
C13 C12 C11 107.1(3) . .
C13 C12 H12 126.4 . .
C11 C12 H12 126.4 . .
C12 C13 C14 106.0(3) . .
C12 C13 H13 127.0 . .
C14 C13 H13 127.0 . .
N2 C14 C13 110.3(3) . .
N2 C14 C15 116.7(2) . .
C13 C14 C15 133.1(3) . .
O4 C15 O5 121.7(3) . .
O4 C15 C14 122.8(3) . .
O5 C15 C14 115.5(2) . .
O5 C16 H16A 109.5 . .
O5 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O5 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
Zn1 O1 Zn1 135.12(15) 2_655 .
Zn1 O1 Zn2 100.627(17) 2_655 .
Zn1 O1 Zn2 100.844(17) . .
Zn1 O1 Zn2 100.847(17) 2_655 2_655
Zn1 O1 Zn2 100.626(17) . 2_655
Zn2 O1 Zn2 121.58(14) . 2_655
C9 O2 Zn1 132.13(18) . .
C9 O2 Zn2 104.33(17) . .
Zn1 O2 Zn2 83.15(6) . .
C9 O3 C10 116.8(2) . .
C15 O4 Zn1 115.56(18) . 2_655
C15 O4 Zn2 103.67(17) . .
Zn1 O4 Zn2 80.19(6) 2_655 .
C15 O5 C16 117.9(2) . .
C5 N1 C8 106.6(2) . .
C5 N1 Zn2 138.0(2) . .
C8 N1 Zn2 115.45(19) . .
C11 N2 C14 105.8(2) . .
C11 N2 Zn2 136.3(2) . .
C14 N2 Zn2 117.38(19) . .
O1 Zn1 C1 141.30(12) . .
O1 Zn1 O2 87.91(7) . .
C1 Zn1 O2 117.80(10) . .
O1 Zn1 O4 89.80(7) . 2_655
C1 Zn1 O4 116.86(11) . 2_655
O2 Zn1 O4 89.58(7) . 2_655
O1 Zn1 Zn2 40.15(3) . 2_655
C1 Zn1 Zn2 142.09(9) . 2_655
O2 Zn1 Zn2 99.22(5) . 2_655
O4 Zn1 Zn2 51.83(5) 2_655 2_655
O1 Zn1 Zn2 40.04(3) . .
C1 Zn1 Zn2 140.78(9) . .
O2 Zn1 Zn2 50.35(5) . .
O4 Zn1 Zn2 101.28(5) 2_655 .
Zn2 Zn1 Zn2 69.802(13) 2_655 .
N1 Zn2 N2 130.69(10) . .
N1 Zn2 O1 116.14(9) . .
N2 Zn2 O1 112.95(10) . .
N1 Zn2 O2 79.45(8) . .
N2 Zn2 O2 102.12(9) . .
O1 Zn2 O2 83.31(5) . .
N1 Zn2 O4 110.99(8) . .
N2 Zn2 O4 77.12(8) . .
O1 Zn2 O4 85.19(5) . .
O2 Zn2 O4 167.12(7) . .
N1 Zn2 Zn1 133.39(7) . 2_655
N2 Zn2 Zn1 89.31(7) . 2_655
O1 Zn2 Zn1 39.22(2) . 2_655
O2 Zn2 Zn1 119.41(5) . 2_655
O4 Zn2 Zn1 47.99(5) . 2_655
N1 Zn2 Zn1 111.28(7) . .
N2 Zn2 Zn1 103.39(7) . .
O1 Zn2 Zn1 39.12(2) . .
O2 Zn2 Zn1 46.50(5) . .
O4 Zn2 Zn1 120.85(5) . .
Zn1 Zn2 Zn1 72.912(14) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C4 1.521(5) .
C1 C2 1.524(5) .
C1 C3 1.535(5) .
C1 Zn1 1.976(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 N1 1.344(4) .
C5 C6 1.398(4) .
C5 H5 0.9500 .
C6 C7 1.392(4) .
C6 H6 0.9500 .
C7 C8 1.394(4) .
C7 H7 0.9500 .
C8 N1 1.382(4) .
C8 C9 1.416(4) .
C9 O2 1.255(3) .
C9 O3 1.331(3) .
C10 O3 1.446(4) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 N2 1.348(4) .
C11 C12 1.396(5) .
C11 H11 0.9500 .
C12 C13 1.386(4) .
C12 H12 0.9500 .
C13 C14 1.395(4) .
C13 H13 0.9500 .
C14 N2 1.387(4) .
C14 C15 1.418(4) .
C15 O4 1.260(3) .
C15 O5 1.333(3) .
C16 O5 1.445(4) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
O1 Zn1 1.9349(11) 2_655
O1 Zn1 1.9349(11) .
O1 Zn2 1.9730(13) .
O1 Zn2 1.9730(13) 2_655
O2 Zn1 2.2007(19) .
O2 Zn2 2.3360(19) .
O4 Zn1 2.268(2) 2_655
O4 Zn2 2.399(2) .
N1 Zn2 1.936(2) .
N2 Zn2 1.948(2) .
Zn1 Zn2 3.0074(4) 2_655
Zn1 Zn2 3.0121(5) .
