#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:05:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180411 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/80/7208051.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_7208051
loop_
_publ_author_name
'Conterosito, Eleonora'
'Croce, Gianluca'
'Palin, Luca'
'Boccaleri, Enrico'
'van Beek, Wouter'
'Milanesio, Marco'
_publ_section_title
;
 Crystal structure and solid-state transformations of
 Zn--triethanolamine--acetate complexes to ZnO
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              4472
_journal_paper_doi               10.1039/c2ce06468e
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C10 H21 N O7 Zn'
_chemical_formula_weight         332.65
_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
_cell_angle_alpha                73.688(7)
_cell_angle_beta                 77.256(7)
_cell_angle_gamma                85.402(6)
_cell_formula_units_Z            2
_cell_length_a                   6.0895(4)
_cell_length_b                   10.4778(9)
_cell_length_c                   11.4086(10)
_cell_measurement_temperature    100(2)
_cell_volume                     681.28(10)
_computing_cell_refinement       'CrysAlisPRO 171.34.44(OXford Diffraction)'
_computing_data_collection       'CrysAlisPRO 171.34.44(OXford Diffraction)'
_computing_data_reduction        'CrysAlisPRO 171.34.44(OXford Diffraction)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, L. J., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2007)'
_computing_structure_solution    'Sir2008 (Burla, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.900
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1748
_diffrn_reflns_av_sigmaI/netI    0.1764
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22337
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.79
_diffrn_reflns_theta_min         4.38
_exptl_absorpt_coefficient_mu    1.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.0945
_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)+(0.1065P)²+2.9092P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2342
_refine_ls_wR_factor_ref         0.2695
_reflns_number_gt                2066
_reflns_number_total             4177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce06468e.txt
_cod_data_source_block           exp_254
_cod_original_cell_volume        681.28(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7208051
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 0.50023(15) 0.29101(10) 0.79139(9) 0.0303(3) Uani 1 1 d .
O6 O 0.0753(9) 0.1759(6) 0.9032(6) 0.0390(14) Uani 1 1 d .
O7 O 0.9862(9) 0.5704(6) 0.7060(6) 0.0403(14) Uani 1 1 d .
O5 O 0.6708(10) 0.1179(6) 0.8865(6) 0.0415(15) Uani 1 1 d .
O4 O 0.7702(9) 0.4011(6) 0.7453(6) 0.0395(14) Uani 1 1 d .
O1 O 0.9858(11) 0.1583(7) 0.3911(6) 0.0529(17) Uani 1 1 d .
H1 H 1.0022 0.2384 0.3592 0.079 Uiso 1 1 calc R
O2 O 0.3318(10) 0.4186(6) 0.6523(6) 0.0407(15) Uani 1 1 d .
O3 O 0.2834(10) 0.3238(6) 0.9329(6) 0.0421(15) Uani 1 1 d .
N1 N 0.5215(10) 0.1718(7) 0.6678(6) 0.0285(14) Uani 1 1 d .
C4 C 0.2936(13) 0.3564(8) 0.5632(8) 0.0351(19) Uani 1 1 d .
H5A H 0.4025 0.3865 0.4855 0.042 Uiso 1 1 calc R
H5B H 0.1440 0.3797 0.5465 0.042 Uiso 1 1 calc R
C9 C 0.6035(15) 0.5981(10) 0.7978(10) 0.048(2) Uani 1 1 d .
H8B H 0.6550 0.6844 0.7916 0.072 Uiso 1 1 calc R
H8C H 0.5439 0.5540 0.8837 0.072 Uiso 1 1 calc R
H8A H 0.4879 0.6075 0.7505 0.072 Uiso 1 1 calc R
C8 C 0.5177(15) 0.0341(8) 0.7473(9) 0.038(2) Uani 1 1 d .
H7A H 0.5476 -0.0270 0.6953 0.046 Uiso 1 1 calc R
H7B H 0.3697 0.0155 0.8007 0.046 Uiso 1 1 calc R
C10 C -0.0900(15) 0.2914(11) 1.0525(9) 0.052(3) Uani 1 1 d .
H9A H -0.0433 0.3583 1.0841 0.077 Uiso 1 1 calc R
H9B H -0.1301 0.2127 1.1197 0.077 Uiso 1 1 calc R
H9C H -0.2178 0.3239 1.0155 0.077 Uiso 1 1 calc R
C5 C 0.7978(12) 0.5169(8) 0.7466(8) 0.0322(18) Uani 1 1 d .
C1 C 0.7727(15) 0.1358(9) 0.4651(9) 0.044(2) Uani 1 1 d .
H2A H 0.7529 0.0409 0.5010 0.052 Uiso 1 1 calc R
H2B H 0.6619 0.1682 0.4136 0.052 Uiso 1 1 calc R
C6 C 0.0987(13) 0.2591(9) 0.9562(8) 0.0354(19) Uani 1 1 d .
C2 C 0.7314(12) 0.2042(9) 0.5698(8) 0.0331(18) Uani 1 1 d .
H3A H 0.8584 0.1831 0.6109 0.040 Uiso 1 1 calc R
H3B H 0.7310 0.2995 0.5321 0.040 Uiso 1 1 calc R
C3 C 0.3161(13) 0.2064(8) 0.6144(8) 0.0342(18) Uani 1 1 d .
H4B H 0.1844 0.1736 0.6785 0.041 Uiso 1 1 calc R
H4A H 0.3247 0.1642 0.5479 0.041 Uiso 1 1 calc R
C7 C 0.6930(15) 0.0136(8) 0.8265(9) 0.038(2) Uani 1 1 d .
H6B H 0.6726 -0.0717 0.8887 0.046 Uiso 1 1 calc R
H6A H 0.8425 0.0141 0.7745 0.046 Uiso 1 1 calc R
H101 H 0.238(17) 0.463(10) 0.675(9) 0.046 Uiso 1 1 d .
H102 H 0.825(17) 0.138(9) 0.866(9) 0.046 Uiso 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'
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
O3 Zn1 O4 112.9(2)
O3 Zn1 N1 136.9(3)
O4 Zn1 N1 110.2(2)
O3 Zn1 O5 99.5(3)
O4 Zn1 O5 92.8(2)
N1 Zn1 O5 79.9(2)
O3 Zn1 O2 95.0(3)
O4 Zn1 O2 95.3(2)
N1 Zn1 O2 79.2(2)
O5 Zn1 O2 159.1(2)
C7 O5 Zn1 112.2(4)
C5 O4 Zn1 132.5(5)
C4 O2 Zn1 113.6(5)
C6 O3 Zn1 112.4(5)
C8 N1 C3 111.7(6)
C8 N1 C2 113.7(6)
C3 N1 C2 111.9(6)
C8 N1 Zn1 104.8(5)
C3 N1 Zn1 105.1(5)
C2 N1 Zn1 109.0(5)
O2 C4 C3 109.0(7)
N1 C8 C7 110.2(7)
O4 C5 O7 121.7(7)
O4 C5 C9 120.7(7)
O7 C5 C9 117.6(7)
O1 C1 C2 112.3(7)
O6 C6 O3 123.1(7)
O6 C6 C10 120.4(8)
O3 C6 C10 116.4(8)
N1 C2 C1 117.8(7)
N1 C3 C4 110.4(6)
O5 C7 C8 109.1(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Zn1 O3 1.941(6)
Zn1 O4 1.973(6)
Zn1 N1 2.109(6)
Zn1 O5 2.153(6)
Zn1 O2 2.160(6)
O6 C6 1.225(10)
O7 C5 1.252(9)
O5 C7 1.427(10)
O4 C5 1.243(9)
O1 C1 1.381(11)
O2 C4 1.420(10)
O3 C6 1.298(10)
N1 C8 1.472(11)
N1 C3 1.486(9)
N1 C2 1.491(10)
C4 C3 1.521(11)
C9 C5 1.509(11)
C8 C7 1.511(11)
C10 C6 1.493(12)
C1 C2 1.524(11)
