#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:51:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179993 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/87/7028786.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_7028786
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            'C26 H52 N4 O4 Zr'
_chemical_formula_weight         575.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 117.329(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5933(13)
_cell_length_b                   9.7100(5)
_cell_length_c                   17.6258(12)
_cell_measurement_reflns_used    3890
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      27.424
_cell_measurement_theta_min      2.937
_cell_volume                     3131.1(4)
_computing_cell_refinement       'CrysAlisPro Version 1.171.34.44'
_computing_data_collection       'CrysAlisPro Version 1.171.34.44'
_computing_data_reduction        'CrysAlisPro Version 1.171.34.44'
_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      104(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '526 images at 1.0 deg. in ω and 40 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  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12209
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abspack
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0331
_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)+(0.0331P)²+0.4768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0782
_reflns_number_gt                2427
_reflns_number_total             2769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52335g.txt
_cod_data_source_block           cvd359
_cod_original_cell_volume        3131.1(3)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7028786
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zr1 Zr 0.0000 0.30674(3) 0.2500 0.01457(11) Uani 1 2 d S
N1 N -0.01036(10) 0.50345(19) 0.32685(11) 0.0168(4) Uani 1 1 d .
C2 C 0.06039(12) 0.5682(2) 0.38165(13) 0.0204(5) Uani 1 1 d .
H2A H 0.0531 0.6673 0.3887 0.024 Uiso 1 1 calc R
H2B H 0.0929 0.5604 0.3544 0.024 Uiso 1 1 calc R
C3 C 0.09603(12) 0.4985(3) 0.46891(14) 0.0241(5) Uani 1 1 d .
H3A H 0.0676 0.5215 0.4998 0.029 Uiso 1 1 calc R
H3B H 0.0936 0.3975 0.4606 0.029 Uiso 1 1 calc R
C4 C 0.17482(13) 0.5395(3) 0.52363(15) 0.0282(6) Uani 1 1 d .
H4A H 0.1960 0.4845 0.5769 0.034 Uiso 1 1 calc R
H4B H 0.2036 0.5212 0.4925 0.034 Uiso 1 1 calc R
O5 O 0.17822(9) 0.68159(17) 0.54366(10) 0.0307(4) Uani 1 1 d .
C6 C 0.24978(14) 0.7217(3) 0.60290(17) 0.0402(7) Uani 1 1 d .
H6A H 0.2658 0.6672 0.6552 0.060 Uiso 1 1 calc R
H6B H 0.2500 0.8196 0.6164 0.060 Uiso 1 1 calc R
H6C H 0.2831 0.7060 0.5781 0.060 Uiso 1 1 calc R
C7 C -0.06803(14) 0.6909(2) 0.36945(16) 0.0295(6) Uani 1 1 d .
H7A H -0.0292 0.6851 0.4284 0.044 Uiso 1 1 calc R
H7B H -0.1152 0.7037 0.3695 0.044 Uiso 1 1 calc R
H7C H -0.0586 0.7690 0.3407 0.044 Uiso 1 1 calc R
C8 C -0.06970(12) 0.5591(2) 0.32265(14) 0.0201(5) Uani 1 1 d .
C9 C -0.14155(12) 0.5025(2) 0.27220(14) 0.0211(5) Uani 1 1 d .
H9 H -0.1805 0.5445 0.2785 0.025 Uiso 1 1 calc R
C10 C -0.15964(12) 0.3954(2) 0.21653(14) 0.0197(5) Uani 1 1 d .
O11 O -0.11214(8) 0.32887(15) 0.20027(9) 0.0184(4) Uani 1 1 d .
C11 C -0.23675(12) 0.3446(3) 0.16806(16) 0.0299(6) Uani 1 1 d .
H11A H -0.2518 0.3482 0.1067 0.045 Uiso 1 1 calc R
H11B H -0.2692 0.4031 0.1811 0.045 Uiso 1 1 calc R
H11C H -0.2397 0.2495 0.1848 0.045 Uiso 1 1 calc R
N13 N 0.00547(10) 0.17087(18) 0.34296(11) 0.0167(4) Uani 1 1 d .
C14 C 0.05447(12) 0.0515(2) 0.36860(14) 0.0233(5) Uani 1 1 d .
H14A H 0.0672 0.0294 0.3222 0.028 Uiso 1 1 calc R
H14B H 0.0282 -0.0288 0.3759 0.028 Uiso 1 1 calc R
C15 C 0.12434(13) 0.0737(3) 0.45068(15) 0.0359(7) Uani 1 1 d .
H15A H 0.1535 0.1460 0.4420 0.054 Uiso 1 1 calc R
H15B H 0.1525 -0.0121 0.4670 0.054 Uiso 1 1 calc R
H15C H 0.1122 0.1016 0.4961 0.054 Uiso 1 1 calc R
C16 C -0.03778(13) 0.1810(2) 0.38919(15) 0.0223(5) Uani 1 1 d .
H16A H -0.0538 0.2776 0.3872 0.027 Uiso 1 1 calc R
H16B H -0.0063 0.1570 0.4498 0.027 Uiso 1 1 calc R
C17 C -0.10469(13) 0.0883(3) 0.35412(18) 0.0343(6) Uani 1 1 d .
H17A H -0.1354 0.1088 0.2935 0.051 Uiso 1 1 calc R
H17B H -0.1326 0.1045 0.3857 0.051 Uiso 1 1 calc R
H17C H -0.0892 -0.0083 0.3605 0.051 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
N13 Zr1 N13 100.63(10) 2 .
N13 Zr1 O11 94.96(6) 2 .
N13 Zr1 O11 92.64(6) . .
N13 Zr1 O11 92.64(6) 2 2
N13 Zr1 O11 94.96(6) . 2
O11 Zr1 O11 168.09(8) . 2
N13 Zr1 N1 165.10(6) 2 .
N13 Zr1 N1 92.70(7) . .
O11 Zr1 N1 77.65(6) . .
O11 Zr1 N1 92.82(6) 2 .
N13 Zr1 N1 92.70(7) 2 2
N13 Zr1 N1 165.10(6) . 2
O11 Zr1 N1 92.82(6) . 2
O11 Zr1 N1 77.65(6) 2 2
N1 Zr1 N1 74.97(8) . 2
C8 N1 C2 118.65(19) . .
C8 N1 Zr1 128.21(15) . .
C2 N1 Zr1 113.09(13) . .
N1 C2 C3 110.23(18) . .
N1 C2 H2A 109.6 . .
C3 C2 H2A 109.6 . .
N1 C2 H2B 109.6 . .
C3 C2 H2B 109.6 . .
H2A C2 H2B 108.1 . .
C4 C3 C2 113.9(2) . .
C4 C3 H3A 108.8 . .
C2 C3 H3A 108.8 . .
C4 C3 H3B 108.8 . .
C2 C3 H3B 108.8 . .
H3A C3 H3B 107.7 . .
O5 C4 C3 109.33(19) . .
O5 C4 H4A 109.8 . .
C3 C4 H4A 109.8 . .
O5 C4 H4B 109.8 . .
C3 C4 H4B 109.8 . .
H4A C4 H4B 108.3 . .
C6 O5 C4 111.55(19) . .
O5 C6 H6A 109.5 . .
O5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
O5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C8 C7 H7A 109.5 . .
C8 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C8 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N1 C8 C9 123.1(2) . .
N1 C8 C7 122.1(2) . .
C9 C8 C7 114.8(2) . .
C10 C9 C8 127.0(2) . .
C10 C9 H9 116.5 . .
C8 C9 H9 116.5 . .
O11 C10 C9 123.4(2) . .
O11 C10 C11 114.6(2) . .
C9 C10 C11 122.0(2) . .
C10 O11 Zr1 139.35(14) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C16 N13 C14 113.01(18) . .
C16 N13 Zr1 125.06(14) . .
C14 N13 Zr1 121.92(14) . .
N13 C14 C15 113.5(2) . .
N13 C14 H14A 108.9 . .
C15 C14 H14A 108.9 . .
N13 C14 H14B 108.9 . .
C15 C14 H14B 108.9 . .
H14A C14 H14B 107.7 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
N13 C16 C17 113.88(19) . .
N13 C16 H16A 108.8 . .
C17 C16 H16A 108.8 . .
N13 C16 H16B 108.8 . .
C17 C16 H16B 108.8 . .
H16A C16 H16B 107.7 . .
C16 C17 H17A 109.5 . .
C16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C16 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 N13 2.0660(18) 2
Zr1 N13 2.0660(18) .
Zr1 O11 2.0710(14) .
Zr1 O11 2.0710(14) 2
Zr1 N1 2.4070(18) .
Zr1 N1 2.4070(18) 2
N1 C8 1.307(3) .
N1 C2 1.469(3) .
C2 C3 1.525(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.511(3) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 O5 1.418(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
O5 C6 1.414(3) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.514(3) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 C9 1.440(3) .
C9 C10 1.360(3) .
C9 H9 0.9500 .
C10 O11 1.309(3) .
C10 C11 1.499(3) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
N13 C16 1.460(3) .
N13 C14 1.465(3) .
C14 C15 1.516(3) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 C17 1.520(3) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
