#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:34:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180227 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/13/7111333.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7111333
loop_
_publ_author_name
'Spijksma, Gerald I.'
'Bouwmeester, Henny J. M.'
'Blank, Dave H. A.'
'Kessler, Vadim G.'
_publ_section_title
;
 Stabilization and destabilization of zirconium propoxide precursors by
 acetylacetoneElectronic supplementary information (ESI) available:
 summary of 1H NMR spectra and CIF files for compounds 1 and 2. See
 http://www.rsc.org/suppdata/cc/b4/b406012a/
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1874
_journal_page_last               1875
_journal_paper_doi               10.1039/b406012a
_journal_year                    2004
_chemical_formula_sum            'C28 H56 O10 Zr2'
_chemical_formula_weight         735.17
_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                87.74(4)
_cell_angle_beta                 67.16(3)
_cell_angle_gamma                64.75(5)
_cell_formula_units_Z            1
_cell_length_a                   10.004(16)
_cell_length_b                   10.686(14)
_cell_length_c                   12.27(2)
_cell_measurement_reflns_used    998(I>10sigma(I))
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      1.82
_cell_volume                     1081(3)
_computing_cell_refinement       'Bruker SAINTPLUS'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL-NT'
_computing_publication_material  'Bruker SHELXTL-NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type  'Bruker SMART CCD 1k'
_diffrn_measurement_method       'Bruker SMART'
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0821
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5584
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.9261
_exptl_absorpt_correction_T_min  0.7810
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.879
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0469
_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)+(0.0589P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                2261
_reflns_number_total             4123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b406012asup1.cif
_cod_data_source_block           zrac1m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111333
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 -0.13832(5) 0.07918(4) 0.15214(4) 0.06444(19) Uani 1 1 d .
O1 O 0.1136(3) -0.0054(3) 0.0344(2) 0.0648(7) Uani 1 1 d .
O2 O -0.1310(4) 0.1642(3) 0.2927(3) 0.0901(9) Uani 1 1 d .
O3 O -0.4021(4) 0.1880(3) 0.2148(3) 0.0877(9) Uani 1 1 d .
O4 O -0.1809(4) 0.2826(3) 0.0767(3) 0.0867(9) Uani 1 1 d .
O5 O -0.1532(4) -0.0877(3) 0.2164(3) 0.0898(9) Uani 1 1 d .
C2 C -0.5073(6) 0.3192(6) 0.2233(5) 0.0919(15) Uani 1 1 d .
C3 C -0.4639(8) 0.4235(6) 0.1705(6) 0.1126(19) Uani 1 1 d .
H2A H -0.5463 0.5138 0.1845 0.135 Uiso 1 1 calc R
C6 C 0.2536(6) -0.0120(6) 0.0565(5) 0.1009(17) Uani 1 1 d .
H3A H 0.3503 -0.0614 -0.0175 0.121 Uiso 1 1 calc R
C4 C -0.3051(8) 0.4002(5) 0.0984(5) 0.0920(15) Uani 1 1 d .
C62 C 0.2382(8) 0.1351(7) 0.0735(6) 0.156(3) Uani 1 1 d .
H5A H 0.2221 0.1817 0.0079 0.234 Uiso 1 1 calc R
H5B H 0.3354 0.1290 0.0762 0.234 Uiso 1 1 calc R
H5C H 0.1473 0.1872 0.1470 0.234 Uiso 1 1 calc R
C1 C -0.6851(7) 0.3489(7) 0.3001(6) 0.144(3) Uani 1 1 d .
H6A H -0.6885 0.2640 0.3262 0.216 Uiso 1 1 calc R
H6B H -0.7474 0.3834 0.2532 0.216 Uiso 1 1 calc R
H6C H -0.7297 0.4177 0.3684 0.216 Uiso 1 1 calc R
C5 C -0.2722(9) 0.5225(5) 0.0435(6) 0.148(3) Uani 1 1 d .
H7A H -0.1582 0.4892 -0.0038 0.223 Uiso 1 1 calc R
H7B H -0.3082 0.5951 0.1064 0.223 Uiso 1 1 calc R
H7C H -0.3300 0.5590 -0.0063 0.223 Uiso 1 1 calc R
C8 C -0.1507(10) 0.2371(8) 0.3998(6) 0.147(3) Uani 1 1 d .
H8A H -0.0432 0.1985 0.4010 0.177 Uiso 1 1 calc R
C61 C 0.2803(9) -0.1010(8) 0.1543(7) 0.160(3) Uani 1 1 d .
H9A H 0.2899 -0.1914 0.1348 0.239 Uiso 1 1 calc R
H9B H 0.1899 -0.0555 0.2297 0.239 Uiso 1 1 calc R
H9C H 0.3778 -0.1118 0.1595 0.239 Uiso 1 1 calc R
C7 C -0.1857(11) -0.1884(10) 0.2802(10) 0.201(4) Uani 1 1 d .
H10 H -0.1459 -0.2566 0.2104 0.241 Uiso 1 1 calc R
C82 C -0.1960(18) 0.3814(10) 0.3883(9) 0.299(8) Uani 1 1 d .
H11A H -0.2090 0.4300 0.4586 0.449 Uiso 1 1 calc R
H11B H -0.2964 0.4217 0.3791 0.449 Uiso 1 1 calc R
H11C H -0.1130 0.3895 0.3194 0.449 Uiso 1 1 calc R
C72 C -0.0706(14) -0.2749(12) 0.3268(12) 0.318(9) Uani 1 1 d .
H12A H 0.0335 -0.2786 0.2792 0.477 Uiso 1 1 calc R
H12B H -0.0623 -0.3677 0.3245 0.477 Uiso 1 1 calc R
H12C H -0.1062 -0.2361 0.4080 0.477 Uiso 1 1 calc R
C71 C -0.3489(12) -0.1655(12) 0.3254(10) 0.261(6) Uani 1 1 d .
H13A H -0.4020 -0.1040 0.2804 0.392 Uiso 1 1 calc R
H13B H -0.4032 -0.1238 0.4079 0.392 Uiso 1 1 calc R
H13C H -0.3522 -0.2532 0.3186 0.392 Uiso 1 1 calc R
C81 C -0.2505(18) 0.2133(15) 0.5040(8) 0.346(11) Uani 1 1 d .
H14A H -0.2101 0.1145 0.5061 0.519 Uiso 1 1 calc R
H14B H -0.3582 0.2507 0.5073 0.519 Uiso 1 1 calc R
H14C H -0.2528 0.2583 0.5714 0.519 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'
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
O5 Zr1 O2 98.01(17) . .
O5 Zr1 O1 101.46(14) . .
O2 Zr1 O1 98.60(16) . .
O5 Zr1 O3 90.14(15) . .
O2 Zr1 O3 95.64(15) . .
O1 Zr1 O3 160.13(12) . .
O5 Zr1 O4 165.67(13) . .
O2 Zr1 O4 89.35(16) . .
O1 Zr1 O4 89.48(13) . .
O3 Zr1 O4 76.86(13) . .
O5 Zr1 O1 92.89(15) . 2
O2 Zr1 O1 167.54(11) . 2
O1 Zr1 O1 73.19(14) . 2
O3 Zr1 O1 90.33(12) . 2
O4 Zr1 O1 81.35(14) . 2
O5 Zr1 Zr1 98.69(13) . 2
O2 Zr1 Zr1 136.32(14) . 2
O1 Zr1 Zr1 38.44(7) . 2
O3 Zr1 Zr1 124.31(10) . 2
O4 Zr1 Zr1 84.09(13) . 2
O1 Zr1 Zr1 34.75(10) 2 2
C6 O1 Zr1 129.9(3) . .
C6 O1 Zr1 123.2(3) . 2
Zr1 O1 Zr1 106.81(14) . 2
C8 O2 Zr1 171.8(4) . .
C2 O3 Zr1 134.1(3) . .
C4 O4 Zr1 134.1(4) . .
C7 O5 Zr1 169.6(5) . .
O3 C2 C3 124.2(5) . .
O3 C2 C1 113.2(5) . .
C3 C2 C1 122.7(5) . .
C4 C3 C2 124.4(5) . .
O1 C6 C62 110.1(4) . .
O1 C6 C61 111.9(5) . .
C62 C6 C61 116.0(5) . .
O4 C4 C3 123.9(5) . .
O4 C4 C5 116.3(5) . .
C3 C4 C5 119.8(5) . .
C81 C8 C82 114.6(9) . .
C81 C8 O2 113.1(7) . .
C82 C8 O2 109.1(7) . .
O5 C7 C71 115.3(8) . .
O5 C7 C72 116.7(7) . .
C71 C7 C72 124.5(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O5 1.962(4) .
Zr1 O2 2.022(4) .
Zr1 O1 2.142(4) .
Zr1 O3 2.187(5) .
Zr1 O4 2.264(4) .
Zr1 O1 2.337(5) 2
Zr1 Zr1 3.598(6) 2
O1 C6 1.500(6) .
O1 Zr1 2.337(5) 2
O2 C8 1.456(7) .
O3 C2 1.324(6) .
O4 C4 1.277(6) .
O5 C7 1.382(7) .
C2 C3 1.410(8) .
C2 C1 1.546(7) .
C3 C4 1.399(8) .
C6 C62 1.527(8) .
C6 C61 1.536(8) .
C4 C5 1.548(7) .
C8 C81 1.378(11) .
C8 C82 1.428(11) .
C7 C71 1.414(11) .
C7 C72 1.439(12) .
