#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:51:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179993 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/87/7028789.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_7028789
loop_
_publ_author_name
'Banerjee, Manish'
'Seidel, Rüdiger W'
'Winter, Manuela'
'Becker, Hans-Werner'
'Rogalla, Detlef'
'Devi, Anjana'
_publ_section_title
;
 Novel β-ketoiminato complexes of zirconium: synthesis, characterization
 and evaluation for solution based processing of ZrO2 thin films.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2384
_journal_page_last               2396
_journal_paper_doi               10.1039/c3dt52335g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C34 H70 N2 O10 Zr2'
_chemical_formula_weight         849.36
_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                110.312(8)
_cell_angle_beta                 96.841(7)
_cell_angle_gamma                113.111(7)
_cell_formula_units_Z            1
_cell_length_a                   9.9999(8)
_cell_length_b                   10.4571(8)
_cell_length_c                   12.1982(12)
_cell_measurement_reflns_used    1059
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      26.306
_cell_measurement_theta_min      3.235
_cell_volume                     1050.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.35.11, Agilent Techn.'
_computing_data_collection       'CrysAlisPro 1.171.35.11, Agilent Techn.'
_computing_data_reduction        'CrysAlisPro 1.171.35.11, Agilent Techn.'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      111(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '501 images at 1.0 deg. in ω and 60 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_av_sigmaI/netI    0.1348
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8218
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.546
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.950
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abspack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0439P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                2775
_reflns_number_total             3908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52335g.txt
_cod_data_source_block           cvd422
_cod_original_cell_volume        1050.92(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028789
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
Zr1 Zr -0.03159(7) 0.92985(7) 0.33820(5) 0.0233(2) Uani 1 1 d .
O1 O -0.1802(5) 0.7193(4) 0.2970(4) 0.0402(12) Uani 1 1 d .
N1 N 0.1962(6) 1.1381(6) 0.3618(5) 0.0388(14) Uani 1 1 d .
C1 C -0.2571(11) 0.5668(8) 0.2096(8) 0.085(3) Uani 1 1 d .
H1A H -0.2099 0.5740 0.1428 0.102 Uiso 1 1 calc R
O2 O 0.1058(4) 0.9653(4) 0.5123(3) 0.0264(9) Uani 1 1 d .
C2 C -0.2043(9) 0.4680(8) 0.2454(7) 0.061(2) Uani 1 1 d .
H2A H -0.0946 0.5080 0.2569 0.092 Uiso 1 1 calc R
H2B H -0.2583 0.3622 0.1808 0.092 Uiso 1 1 calc R
H2C H -0.2253 0.4688 0.3220 0.092 Uiso 1 1 calc R
O3 O -0.1337(4) 0.9728(4) 0.2214(3) 0.0294(10) Uani 1 1 d .
C3 C -0.4047(11) 0.5109(10) 0.1512(10) 0.120(4) Uani 1 1 d .
H3A H -0.4644 0.5039 0.2090 0.180 Uiso 1 1 calc R
H3B H -0.4416 0.4083 0.0846 0.180 Uiso 1 1 calc R
H3C H -0.4157 0.5799 0.1174 0.180 Uiso 1 1 calc R
O4 O 0.0725(5) 0.8265(5) 0.2267(4) 0.0394(11) Uani 1 1 d .
C4 C 0.2388(7) 0.9399(8) 0.5164(6) 0.0352(16) Uani 1 1 d .
H4 H 0.2539 0.9164 0.4334 0.042 Uiso 1 1 calc R
O5 O 0.2620(6) 1.4234(6) 0.3188(5) 0.0571(14) Uani 1 1 d .
C5 C 0.2062(8) 0.7987(8) 0.5389(7) 0.052(2) Uani 1 1 d .
H5A H 0.1938 0.8187 0.6207 0.078 Uiso 1 1 calc R
H5B H 0.2912 0.7746 0.5332 0.078 Uiso 1 1 calc R
H5C H 0.1126 0.7112 0.4774 0.078 Uiso 1 1 calc R
C6 C 0.3787(7) 1.0824(8) 0.6054(6) 0.0452(18) Uani 1 1 d .
H6A H 0.3913 1.1680 0.5845 0.068 Uiso 1 1 calc R
H6B H 0.4677 1.0648 0.6018 0.068 Uiso 1 1 calc R
H6C H 0.3688 1.1077 0.6883 0.068 Uiso 1 1 calc R
C7 C -0.1802(7) 0.9803(7) 0.1100(5) 0.0347(16) Uani 1 1 d .
H7 H -0.1063 1.0816 0.1153 0.042 Uiso 1 1 calc R
C8 C -0.3335(8) 0.9713(9) 0.0909(6) 0.050(2) Uani 1 1 d .
H8A H -0.4078 0.8727 0.0856 0.075 Uiso 1 1 calc R
H8B H -0.3621 0.9792 0.0147 0.075 Uiso 1 1 calc R
H8C H -0.3320 1.0561 0.1597 0.075 Uiso 1 1 calc R
C9 C -0.1739(8) 0.8540(8) 0.0062(6) 0.0454(18) Uani 1 1 d .
H9A H -0.0702 0.8660 0.0216 0.068 Uiso 1 1 calc R
H9B H -0.2028 0.8603 -0.0707 0.068 Uiso 1 1 calc R
H9C H -0.2446 0.7535 0.0003 0.068 Uiso 1 1 calc R
C10 C 0.1907(10) 0.7250(9) 0.0912(6) 0.070(3) Uani 1 1 d .
H10A H 0.1730 0.6424 0.1172 0.105 Uiso 1 1 calc R
H10B H 0.2888 0.7575 0.0739 0.105 Uiso 1 1 calc R
H10C H 0.1091 0.6871 0.0171 0.105 Uiso 1 1 calc R
C11 C 0.1922(8) 0.8560(8) 0.1887(6) 0.0418(17) Uani 1 1 d .
C12 C 0.3115(8) 1.0019(8) 0.2351(7) 0.0488(19) Uani 1 1 d .
H12 H 0.3978 1.0138 0.2064 0.059 Uiso 1 1 calc R
C13 C 0.3164(8) 1.1391(9) 0.3245(7) 0.0458(19) Uani 1 1 d .
C14 C 0.4662(8) 1.2851(8) 0.3706(8) 0.063(2) Uani 1 1 d .
H14A H 0.4484 1.3646 0.3567 0.094 Uiso 1 1 calc R
H14B H 0.5364 1.2637 0.3265 0.094 Uiso 1 1 calc R
H14C H 0.5107 1.3212 0.4583 0.094 Uiso 1 1 calc R
C15 C 0.2072(8) 1.2844(7) 0.4417(6) 0.050(2) Uani 1 1 d .
H15A H 0.3144 1.3549 0.4925 0.060 Uiso 1 1 calc R
H15B H 0.1450 1.2672 0.4975 0.060 Uiso 1 1 calc R
C16 C 0.1550(7) 1.3616(7) 0.3740(6) 0.0394(17) Uani 1 1 d .
H16A H 0.0563 1.2853 0.3107 0.047 Uiso 1 1 calc R
H16B H 0.1400 1.4447 0.4321 0.047 Uiso 1 1 calc R
C17 C 0.2117(9) 1.4860(9) 0.2452(7) 0.063(2) Uani 1 1 d .
H17A H 0.1164 1.4053 0.1815 0.095 Uiso 1 1 calc R
H17B H 0.2894 1.5251 0.2069 0.095 Uiso 1 1 calc R
H17C H 0.1948 1.5704 0.2967 0.095 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'
Zr Zr -2.9673 0.5597 '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
O3 Zr1 O1 100.73(17) . .
O3 Zr1 O4 97.72(17) . .
O1 Zr1 O4 84.59(18) . .
O3 Zr1 O2 95.86(15) . 2_576
O1 Zr1 O2 95.00(16) . 2_576
O4 Zr1 O2 166.25(16) . 2_576
O3 Zr1 O2 159.85(15) . .
O1 Zr1 O2 95.01(16) . .
O4 Zr1 O2 96.20(15) . .
O2 Zr1 O2 70.12(16) 2_576 .
O3 Zr1 N1 87.87(17) . .
O1 Zr1 N1 159.80(19) . .
O4 Zr1 N1 76.10(18) . .
O2 Zr1 N1 102.33(17) 2_576 .
O2 Zr1 N1 81.41(16) . .
O3 Zr1 Zr1 129.96(12) . 2_576
O1 Zr1 Zr1 96.12(13) . 2_576
O4 Zr1 Zr1 130.74(12) . 2_576
O2 Zr1 Zr1 35.57(10) 2_576 2_576
O2 Zr1 Zr1 34.55(9) . 2_576
N1 Zr1 Zr1 92.09(13) . 2_576
C1 O1 Zr1 146.9(5) . .
C13 N1 C15 118.1(6) . .
C13 N1 Zr1 130.1(5) . .
C15 N1 Zr1 111.3(4) . .
C3 C1 O1 117.5(8) . .
C3 C1 C2 120.2(8) . .
O1 C1 C2 111.6(7) . .
C3 C1 H1A 101.0 . .
O1 C1 H1A 101.0 . .
C2 C1 H1A 101.0 . .
C4 O2 Zr1 129.0(3) . 2_576
C4 O2 Zr1 120.5(3) . .
Zr1 O2 Zr1 109.88(16) 2_576 .
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 . .
C7 O3 Zr1 159.2(4) . .
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 . .
C11 O4 Zr1 142.9(4) . .
O2 C4 C6 111.1(5) . .
O2 C4 C5 109.1(5) . .
C6 C4 C5 114.7(5) . .
O2 C4 H4 107.2 . .
C6 C4 H4 107.2 . .
C5 C4 H4 107.2 . .
C16 O5 C17 112.7(6) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
O3 C7 C8 111.0(5) . .
O3 C7 C9 108.9(5) . .
C8 C7 C9 112.3(5) . .
O3 C7 H7 108.2 . .
C8 C7 H7 108.2 . .
C9 C7 H7 108.2 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 H10A 109.5 . .
C11 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C11 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O4 C11 C12 122.0(7) . .
O4 C11 C10 116.0(7) . .
C12 C11 C10 122.0(7) . .
C11 C12 C13 125.3(7) . .
C11 C12 H12 117.4 . .
C13 C12 H12 117.4 . .
N1 C13 C12 122.2(6) . .
N1 C13 C14 122.1(7) . .
C12 C13 C14 115.6(6) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N1 C15 C16 113.8(6) . .
N1 C15 H15A 108.8 . .
C16 C15 H15A 108.8 . .
N1 C15 H15B 108.8 . .
C16 C15 H15B 108.8 . .
H15A C15 H15B 107.7 . .
O5 C16 C15 110.8(6) . .
O5 C16 H16A 109.5 . .
C15 C16 H16A 109.5 . .
O5 C16 H16B 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 108.1 . .
O5 C17 H17A 109.5 . .
O5 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
O5 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O3 1.932(4) .
Zr1 O1 1.948(4) .
Zr1 O4 2.074(4) .
Zr1 O2 2.157(4) 2_576
Zr1 O2 2.212(4) .
Zr1 N1 2.351(5) .
Zr1 Zr1 3.5764(12) 2_576
O1 C1 1.390(7) .
N1 C13 1.333(8) .
N1 C15 1.453(8) .
C1 C3 1.346(11) .
C1 C2 1.491(10) .
C1 H1A 1.0000 .
O2 C4 1.453(7) .
O2 Zr1 2.157(4) 2_576
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
O3 C7 1.421(7) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
O4 C11 1.299(7) .
C4 C6 1.495(8) .
C4 C5 1.513(9) .
C4 H4 1.0000 .
O5 C16 1.394(7) .
O5 C17 1.431(8) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.483(8) .
C7 C9 1.509(8) .
C7 H7 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.463(9) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.372(9) .
C12 C13 1.447(10) .
C12 H12 0.9500 .
C13 C14 1.516(9) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C16 1.515(9) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
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
O3 Zr1 O1 C1 64.5(9) . .
O4 Zr1 O1 C1 -32.3(9) . .
O2 Zr1 O1 C1 161.5(9) 2_576 .
O2 Zr1 O1 C1 -128.1(9) . .
N1 Zr1 O1 C1 -49.4(11) . .
Zr1 Zr1 O1 C1 -162.8(9) 2_576 .
O3 Zr1 N1 C13 -108.3(6) . .
O1 Zr1 N1 C13 7.7(9) . .
O4 Zr1 N1 C13 -9.8(6) . .
O2 Zr1 N1 C13 156.1(6) 2_576 .
O2 Zr1 N1 C13 88.8(6) . .
Zr1 Zr1 N1 C13 121.7(6) 2_576 .
O3 Zr1 N1 C15 79.3(4) . .
O1 Zr1 N1 C15 -164.7(5) . .
O4 Zr1 N1 C15 177.8(4) . .
O2 Zr1 N1 C15 -16.2(4) 2_576 .
O2 Zr1 N1 C15 -83.5(4) . .
Zr1 Zr1 N1 C15 -50.6(4) 2_576 .
Zr1 O1 C1 C3 -105.9(12) . .
Zr1 O1 C1 C2 109.5(9) . .
O3 Zr1 O2 C4 -123.5(5) . .
O1 Zr1 O2 C4 95.1(4) . .
O4 Zr1 O2 C4 10.0(4) . .
O2 Zr1 O2 C4 -171.4(5) 2_576 .
N1 Zr1 O2 C4 -64.9(4) . .
Zr1 Zr1 O2 C4 -171.4(5) 2_576 .
O3 Zr1 O2 Zr1 47.9(5) . 2_576
O1 Zr1 O2 Zr1 -93.51(19) . 2_576
O4 Zr1 O2 Zr1 -178.60(18) . 2_576
O2 Zr1 O2 Zr1 0.0 2_576 2_576
N1 Zr1 O2 Zr1 106.5(2) . 2_576
O1 Zr1 O3 C7 -87.9(10) . .
O4 Zr1 O3 C7 -2.0(10) . .
O2 Zr1 O3 C7 175.8(10) 2_576 .
O2 Zr1 O3 C7 131.3(10) . .
N1 Zr1 O3 C7 73.7(10) . .
Zr1 Zr1 O3 C7 164.6(10) 2_576 .
O3 Zr1 O4 C11 85.0(7) . .
O1 Zr1 O4 C11 -174.9(7) . .
O2 Zr1 O4 C11 -86.0(10) 2_576 .
O2 Zr1 O4 C11 -80.4(7) . .
N1 Zr1 O4 C11 -0.9(7) . .
Zr1 Zr1 O4 C11 -81.5(7) 2_576 .
Zr1 O2 C4 C6 -47.8(7) 2_576 .
Zr1 O2 C4 C6 121.8(4) . .
Zr1 O2 C4 C5 79.6(6) 2_576 .
Zr1 O2 C4 C5 -110.8(5) . .
Zr1 O3 C7 C8 150.7(8) . .
Zr1 O3 C7 C9 26.6(13) . .
Zr1 O4 C11 C12 6.7(11) . .
Zr1 O4 C11 C10 -171.9(5) . .
O4 C11 C12 C13 -3.6(11) . .
C10 C11 C12 C13 174.9(7) . .
C15 N1 C13 C12 -173.6(6) . .
Zr1 N1 C13 C12 14.5(10) . .
C15 N1 C13 C14 4.9(9) . .
Zr1 N1 C13 C14 -167.0(5) . .
C11 C12 C13 N1 -6.8(11) . .
C11 C12 C13 C14 174.6(6) . .
C13 N1 C15 C16 90.6(7) . .
Zr1 N1 C15 C16 -96.0(6) . .
C17 O5 C16 C15 175.0(5) . .
N1 C15 C16 O5 -73.7(7) . .
