#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:38:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179800 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/96/7009687.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_7009687
loop_
_publ_author_name
'Chi, Yun'
'Lan, Jing-Wen'
'Ching, Wei-Li'
'Peng, Shie-Ming'
'Lee, Gene-Hsiang'
_publ_section_title
;
 Syntheses and characterization of mixed acetylacetonate--catecholate
 complexes of zirconium, [Zr3(acac)4(cat)4(MeOH)2], [Zr(acac)2(DBcat)]2
 (H2DBcat = 3,5-di-tert-butylcatechol) and
 [Zr4(μ4-O)(acac)4(DBcat)3(OMe)4(MeOH)]
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2923
_journal_paper_doi               10.1039/b002705g
_journal_year                    2000
_chemical_formula_sum            'C48 H68 O12 Zr2'
_chemical_formula_weight         1019.46
_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
_cell_angle_alpha                113.63(3)
_cell_angle_beta                 94.22(3)
_cell_angle_gamma                101.89(3)
_cell_formula_units_Z            1
_cell_length_a                   9.439(2)
_cell_length_b                   11.641(3)
_cell_length_c                   13.567(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.53
_cell_measurement_theta_min      9.37
_cell_volume                     1316.0(7)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        'NRCSDP DATRD2'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       'ω--2θ scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4638
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.7215
_exptl_absorpt_correction_T_min  0.6885
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0051(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_obs          0.0322
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0548P)²+0.4034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0925
_refine_ls_wR_factor_obs         0.0891
_reflns_number_observed          4044
_reflns_number_total             4638
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002705g.txt
_cod_data_source_block           ic6300
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measures' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.4034P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.4034P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1316.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009687
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zr Zr 0.00571(3) 0.16451(2) 0.01788(2) 0.04125(11) Uani 1 d . .
O1 O 0.1655(2) 0.2075(2) -0.06463(15) 0.0518(4) Uani 1 d . .
O2 O 0.0770(2) -0.0133(2) -0.06849(13) 0.0465(4) Uani 1 d . .
O3 O 0.0463(2) 0.3706(2) 0.0732(2) 0.0557(5) Uani 1 d . .
O4 O 0.1506(2) 0.2356(2) 0.16787(15) 0.0513(4) Uani 1 d . .
O5 O -0.1323(2) 0.0954(2) -0.1360(2) 0.0580(5) Uani 1 d . .
O6 O -0.1998(2) 0.2056(2) 0.0596(2) 0.0601(5) Uani 1 d . .
C1 C 0.1888(3) 0.1104(3) -0.1526(2) 0.0467(6) Uani 1 d . .
C2 C 0.2488(3) 0.1257(3) -0.2389(2) 0.0515(7) Uani 1 d . .
C3 C 0.2557(3) 0.0125(3) -0.3271(2) 0.0578(7) Uani 1 d . .
H3A H 0.2961(3) 0.0205(3) -0.3852(2) 0.069 Uiso 1 calc R .
C4 C 0.2060(3) -0.1106(3) -0.3328(2) 0.0560(7) Uani 1 d . .
C5 C 0.1487(3) -0.1223(3) -0.2447(2) 0.0524(7) Uani 1 d . .
H5A H 0.1160(3) -0.2038(3) -0.2454(2) 0.063 Uiso 1 calc R .
C6 C 0.1407(3) -0.0136(3) -0.1570(2) 0.0462(6) Uani 1 d . .
C7 C 0.2963(4) 0.2605(3) -0.2375(3) 0.0655(8) Uani 1 d . .
C8 C 0.1612(5) 0.3138(5) -0.2373(4) 0.0965(13) Uani 1 d . .
H8A H 0.1896(5) 0.3983(5) -0.2364(4) 0.145 Uiso 1 calc R .
H8B H 0.1191(5) 0.3199(5) -0.1736(4) 0.145 Uiso 1 calc R .
H8C H 0.0900(5) 0.2566(5) -0.3017(4) 0.145 Uiso 1 calc R .
C9 C 0.4100(4) 0.3531(4) -0.1338(3) 0.0835(11) Uani 1 d . .
H9A H 0.4952(4) 0.3201(4) -0.1334(3) 0.125 Uiso 1 calc R .
H9B H 0.3676(4) 0.3592(4) -0.0703(3) 0.125 Uiso 1 calc R .
H9C H 0.4381(4) 0.4375(4) -0.1331(3) 0.125 Uiso 1 calc R .
C10 C 0.3653(5) 0.2563(4) -0.3378(4) 0.1007(14) Uani 1 d . .
H10A H 0.4504(5) 0.2230(4) -0.3389(4) 0.151 Uiso 1 calc R .
H10B H 0.3937(5) 0.3424(4) -0.3338(4) 0.151 Uiso 1 calc R .
H10C H 0.2950(5) 0.2011(4) -0.4031(4) 0.151 Uiso 1 calc R .
C11 C 0.2022(4) -0.2339(4) -0.4353(3) 0.0710(9) Uani 1 d . .
C12 C 0.0453(6) -0.3038(6) -0.4868(4) 0.149(3) Uani 1 d . .
H12A H -0.0015(6) -0.2482(6) -0.5062(4) 0.224 Uiso 1 calc R .
H12B H -0.0049(6) -0.3274(6) -0.4359(4) 0.224 Uiso 1 calc R .
H12C H 0.0415(6) -0.3807(6) -0.5512(4) 0.224 Uiso 1 calc R .
C13 C 0.2705(8) -0.3228(6) -0.4066(4) 0.175(3) Uani 1 d . .
H13A H 0.2229(8) -0.3419(6) -0.3528(4) 0.263 Uiso 1 calc R .
H13B H 0.3731(8) -0.2822(6) -0.3776(4) 0.263 Uiso 1 calc R .
H13C H 0.2598(8) -0.4019(6) -0.4708(4) 0.263 Uiso 1 calc R .
C14 C 0.2764(10) -0.2042(6) -0.5192(5) 0.217(5) Uani 1 d . .
H14A H 0.2322(10) -0.1467(6) -0.5378(5) 0.325 Uiso 1 calc R .
H14B H 0.2657(10) -0.2833(6) -0.5833(5) 0.325 Uiso 1 calc R .
H14C H 0.3789(10) -0.1636(6) -0.4902(5) 0.325 Uiso 1 calc R .
C15 C 0.1680(4) 0.5899(3) 0.1266(4) 0.0829(11) Uani 1 d . .
H15A H 0.0927(4) 0.5791(3) 0.0697(4) 0.124 Uiso 1 calc R .
H15B H 0.2628(4) 0.6145(3) 0.1089(4) 0.124 Uiso 1 calc R .
H15C H 0.1590(4) 0.6564(3) 0.1944(4) 0.124 Uiso 1 calc R .
C16 C 0.1518(3) 0.4650(3) 0.1371(3) 0.0541(7) Uani 1 d . .
C17 C 0.2477(3) 0.4555(3) 0.2138(3) 0.0644(8) Uani 1 d . .
H17A H 0.3218(3) 0.5292(3) 0.2581(3) 0.077 Uiso 1 calc R .
C18 C 0.2413(3) 0.3454(3) 0.2294(2) 0.0543(7) Uani 1 d . .
C19 C 0.3413(4) 0.3468(4) 0.3201(3) 0.0880(12) Uani 1 d . .
H19A H 0.3212(4) 0.2617(4) 0.3183(3) 0.132 Uiso 1 calc R .
H19B H 0.3257(4) 0.4074(4) 0.3887(3) 0.132 Uiso 1 calc R .
H19C H 0.4415(4) 0.3723(4) 0.3119(3) 0.132 Uiso 1 calc R .
C20 C -0.3138(5) 0.0146(4) -0.2918(3) 0.1004(14) Uani 1 d . .
H20A H -0.2297(5) -0.0011(4) -0.3257(3) 0.151 Uiso 1 calc R .
H20B H -0.3534(5) 0.0728(4) -0.3127(3) 0.151 Uiso 1 calc R .
H20C H -0.3871(5) -0.0660(4) -0.3150(3) 0.151 Uiso 1 calc R .
C21 C -0.2688(4) 0.0741(3) -0.1699(3) 0.0623(8) Uani 1 d . .
C22 C -0.3696(4) 0.1061(4) -0.1019(3) 0.0732(9) Uani 1 d . .
H22A H -0.4684(4) 0.0814(4) -0.1329(3) 0.088 Uiso 1 calc R .
C23 C -0.3310(3) 0.1728(3) 0.0093(3) 0.0636(8) Uani 1 d . .
C24 C -0.4442(4) 0.2140(5) 0.0791(4) 0.0977(14) Uani 1 d . .
H24A H -0.3980(4) 0.2593(5) 0.1545(4) 0.147 Uiso 1 calc R .
H24B H -0.5191(4) 0.1387(5) 0.0692(4) 0.147 Uiso 1 calc R .
H24C H -0.4879(4) 0.2702(5) 0.0582(4) 0.147 Uiso 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
_geom_angle_publ_flag
O1 Zr O4 94.64(8) . . ?
O1 Zr O5 82.91(8) . . ?
O4 Zr O5 177.55(7) . . ?
O1 Zr O3 76.42(8) . . ?
O4 Zr O3 77.85(8) . . ?
O5 Zr O3 101.47(8) . . ?
O1 Zr O6 140.50(8) . . ?
O4 Zr O6 105.98(8) . . ?
O5 Zr O6 76.03(8) . . ?
O3 Zr O6 75.57(8) . . ?
O1 Zr O2 137.86(7) . 2 ?
O4 Zr O2 80.44(8) . 2 ?
O5 Zr O2 101.40(8) . 2 ?
O3 Zr O2 140.82(7) . 2 ?
O6 Zr O2 79.66(8) . 2 ?
O1 Zr O2 72.43(7) . . ?
O4 Zr O2 97.56(8) . . ?
O5 Zr O2 81.76(8) . . ?
O3 Zr O2 148.05(7) . . ?
O6 Zr O2 134.94(8) . . ?
O2 Zr O2 66.90(7) 2 . ?
O1 Zr Zr 104.90(6) . 2 ?
O4 Zr Zr 88.92(6) . 2 ?
O5 Zr Zr 91.75(7) . 2 ?
O3 Zr Zr 166.77(5) . 2 ?
O6 Zr Zr 108.74(6) . 2 ?
O2 Zr Zr 33.84(5) 2 2 ?
O2 Zr Zr 33.06(4) . 2 ?
C1 O1 Zr 118.6(2) . . ?
C6 O2 Zr 132.5(2) . 2 ?
C6 O2 Zr 113.0(2) . . ?
Zr O2 Zr 113.10(7) 2 . ?
C16 O3 Zr 132.6(2) . . ?
C18 O4 Zr 134.0(2) . . ?
C21 O5 Zr 136.3(2) . . ?
C23 O6 Zr 136.1(2) . . ?
O1 C1 C6 115.4(2) . . ?
O1 C1 C2 124.7(3) . . ?
C6 C1 C2 119.8(3) . . ?
C1 C2 C3 116.7(3) . . ?
C1 C2 C7 120.5(3) . . ?
C3 C2 C7 122.8(3) . . ?
C4 C3 C2 123.8(3) . . ?
C3 C4 C5 118.0(3) . . ?
C3 C4 C11 122.5(3) . . ?
C5 C4 C11 119.3(3) . . ?
C6 C5 C4 119.7(3) . . ?
C5 C6 O2 125.0(2) . . ?
C5 C6 C1 122.0(2) . . ?
O2 C6 C1 112.9(2) . . ?
C8 C7 C2 108.7(3) . . ?
C8 C7 C10 108.6(3) . . ?
C2 C7 C10 112.0(3) . . ?
C8 C7 C9 109.1(3) . . ?
C2 C7 C9 110.1(3) . . ?
C10 C7 C9 108.3(3) . . ?
C13 C11 C14 109.4(5) . . ?
C13 C11 C12 107.9(5) . . ?
C14 C11 C12 107.3(5) . . ?
C13 C11 C4 111.0(3) . . ?
C14 C11 C4 112.4(3) . . ?
C12 C11 C4 108.7(3) . . ?
O3 C16 C17 122.8(3) . . ?
O3 C16 C15 116.6(3) . . ?
C17 C16 C15 120.6(3) . . ?
C18 C17 C16 124.7(3) . . ?
O4 C18 C17 123.0(3) . . ?
O4 C18 C19 115.9(3) . . ?
C17 C18 C19 121.1(3) . . ?
O5 C21 C22 123.8(3) . . ?
O5 C21 C20 115.1(3) . . ?
C22 C21 C20 121.1(3) . . ?
C23 C22 C21 123.0(3) . . ?
O6 C23 C22 123.2(3) . . ?
O6 C23 C24 116.0(3) . . ?
C22 C23 C24 120.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr O1 2.040(2) . ?
Zr O4 2.114(2) . ?
Zr O5 2.127(2) . ?
Zr O3 2.146(2) . ?
Zr O6 2.154(2) . ?
Zr O2 2.159(2) 2 ?
Zr O2 2.204(2) . ?
Zr Zr 3.6400(12) 2 ?
O1 C1 1.345(3) . ?
O2 C6 1.381(3) . ?
O2 Zr 2.159(2) 2 ?
O3 C16 1.268(3) . ?
O4 C18 1.285(3) . ?
O5 C21 1.274(4) . ?
O6 C23 1.272(4) . ?
C1 C6 1.396(4) . ?
C1 C2 1.396(4) . ?
C2 C3 1.398(4) . ?
C2 C7 1.532(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.392(4) . ?
C4 C11 1.538(4) . ?
C5 C6 1.367(4) . ?
C7 C8 1.528(5) . ?
C7 C10 1.539(4) . ?
C7 C9 1.543(5) . ?
C11 C13 1.483(6) . ?
C11 C14 1.496(6) . ?
C11 C12 1.497(6) . ?
C15 C16 1.496(4) . ?
C16 C17 1.381(4) . ?
C17 C18 1.371(4) . ?
C18 C19 1.487(4) . ?
C20 C21 1.501(5) . ?
C21 C22 1.376(5) . ?
C22 C23 1.369(5) . ?
C23 C24 1.506(5) . ?
