#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:58:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179736 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/32/7003275.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_7003275
loop_
_publ_author_name
'Krauzy-Dziedzic, Katarzyna'
'Ejfler, Jolanta'
'Szafert, Sławomir'
'Sobota, Piotr'
_publ_section_title
;
 Titanium and zirconium benzofuranoxides. Crystal structures and
 catalytic properties
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              2620
_journal_page_last               2626
_journal_paper_doi               10.1039/b715048b
_journal_year                    2008
_chemical_formula_sum            'C68 H88 O16 Zr2'
_chemical_formula_weight         1343.82
_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                93.782(5)
_cell_angle_beta                 111.460(5)
_cell_angle_gamma                92.187(4)
_cell_formula_units_Z            1
_cell_length_a                   11.1465(5)
_cell_length_b                   12.1096(7)
_cell_length_c                   13.1966(8)
_cell_measurement_reflns_used    3579
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      36
_cell_measurement_theta_min      3
_cell_volume                     1650.45(17)
_computing_cell_refinement
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_data_collection
'CrysAlis CCD (Oxford Diffraction, 1995-2003)'
_computing_data_reduction
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       'ω 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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19807
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         7632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                6169
_reflns_number_total             7632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715048b.txt
_cod_data_source_block           for_complex_2_kkr4
_cod_original_cell_volume        1650.45(16)
_cod_database_code               7003275
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.44372(2) 0.42182(2) 0.874620(19) 0.01797(8) Uani 1 1 d . . .
O10 O 0.80286(16) 0.26930(17) 0.87371(14) 0.0358(5) Uani 1 1 d . . .
O11 O 0.54072(15) 0.31958(13) 0.81645(13) 0.0223(4) Uani 1 1 d . . .
O20 O 0.42731(16) 0.18752(13) 1.11862(13) 0.0239(4) Uani 1 1 d . . .
O21 O 0.35189(16) 0.31126(14) 0.93276(14) 0.0267(4) Uani 1 1 d . . .
O30 O 0.13590(17) 0.27872(15) 0.57829(13) 0.0327(4) Uani 1 1 d . . .
O31 O 0.30639(16) 0.44343(13) 0.73445(13) 0.0240(4) Uani 1 1 d . . .
O41 O 0.40420(15) 0.55990(13) 0.96349(13) 0.0216(4) Uani 1 1 d . . .
O51 O 0.56333(18) 0.56234(16) 0.84256(16) 0.0313(5) Uani 1 1 d . . .
C11 C 0.5813(2) 0.26182(19) 0.74496(19) 0.0190(5) Uani 1 1 d . . .
C12 C 0.4972(2) 0.2210(2) 0.6414(2) 0.0289(6) Uani 1 1 d . . .
H12 H 0.4101 0.2342 0.6198 0.035 Uiso 1 1 calc R . .
C13 C 0.5399(2) 0.1610(2) 0.5695(2) 0.0327(7) Uani 1 1 d . . .
H13 H 0.4812 0.1346 0.5008 0.039 Uiso 1 1 calc R . .
C14 C 0.6697(2) 0.1396(2) 0.5988(2) 0.0276(6) Uani 1 1 d . . .
H14 H 0.6984 0.0992 0.5507 0.033 Uiso 1 1 calc R . .
C15 C 0.7543(2) 0.1801(2) 0.7012(2) 0.0254(6) Uani 1 1 d . . .
C16 C 0.7102(2) 0.2388(2) 0.77305(19) 0.0209(5) Uani 1 1 d . . .
C17 C 0.8970(3) 0.1699(3) 0.7587(2) 0.0521(9) Uani 1 1 d . . .
H17 H 0.9455 0.2028 0.7191 0.063 Uiso 1 1 calc R . .
H171 H 0.9164 0.0928 0.7665 0.063 Uiso 1 1 calc R . .
C18 C 0.9290(2) 0.2348(2) 0.8724(2) 0.0288(6) Uani 1 1 d . . .
C19 C 1.0109(3) 0.3400(3) 0.8857(3) 0.0517(9) Uani 1 1 d . . .
H19 H 1.0276 0.3775 0.9563 0.078 Uiso 1 1 calc R . .
H191 H 0.9663 0.3871 0.8300 0.078 Uiso 1 1 calc R . .
H192 H 1.0913 0.3227 0.8792 0.078 Uiso 1 1 calc R . .
C110 C 0.9828(3) 0.1630(2) 0.9642(2) 0.0369(7) Uani 1 1 d . . .
H11A H 1.0010 0.2060 1.0325 0.055 Uiso 1 1 calc R . .
H11B H 1.0610 0.1341 0.9622 0.055 Uiso 1 1 calc R . .
H11C H 0.9209 0.1027 0.9569 0.055 Uiso 1 1 calc R . .
C21 C 0.3202(2) 0.2016(2) 0.92247(19) 0.0211(5) Uani 1 1 d . . .
C22 C 0.2466(2) 0.1438(2) 0.8226(2) 0.0279(6) Uani 1 1 d . . .
H22 H 0.2182 0.1815 0.7598 0.034 Uiso 1 1 calc R . .
C23 C 0.2152(3) 0.0311(2) 0.8156(2) 0.0348(7) Uani 1 1 d . . .
H23 H 0.1642 -0.0053 0.7484 0.042 Uiso 1 1 calc R . .
C24 C 0.2582(2) -0.0285(2) 0.9070(2) 0.0318(6) Uani 1 1 d . . .
H24 H 0.2378 -0.1044 0.9015 0.038 Uiso 1 1 calc R . .
C25 C 0.3324(2) 0.0279(2) 1.0069(2) 0.0237(5) Uani 1 1 d . . .
C26 C 0.3585(2) 0.1406(2) 1.01370(19) 0.0206(5) Uani 1 1 d . . .
C27 C 0.3997(3) -0.0095(2) 1.1195(2) 0.0295(6) Uani 1 1 d . . .
H27 H 0.4794 -0.0431 1.1253 0.035 Uiso 1 1 calc R . .
H271 H 0.3445 -0.0621 1.1377 0.035 Uiso 1 1 calc R . .
C28 C 0.4268(2) 0.1004(2) 1.1938(2) 0.0274(6) Uani 1 1 d . . .
C29 C 0.5559(3) 0.1117(3) 1.2862(2) 0.0376(7) Uani 1 1 d . . .
H29 H 0.5654 0.1818 1.3277 0.056 Uiso 1 1 calc R . .
H291 H 0.6233 0.1077 1.2573 0.056 Uiso 1 1 calc R . .
H292 H 0.5615 0.0528 1.3326 0.056 Uiso 1 1 calc R . .
C210 C 0.3161(3) 0.1208(2) 1.2325(2) 0.0330(6) Uani 1 1 d . . .
H21A H 0.3347 0.1893 1.2780 0.049 Uiso 1 1 calc R . .
H21B H 0.3060 0.0609 1.2736 0.049 Uiso 1 1 calc R . .
H21C H 0.2377 0.1249 1.1705 0.049 Uiso 1 1 calc R . .
C31 C 0.2462(2) 0.4628(2) 0.6278(2) 0.0259(6) Uani 1 1 d . . .
C32 C 0.2643(3) 0.5625(2) 0.5877(2) 0.0392(7) Uani 1 1 d . . .
H32 H 0.3188 0.6193 0.6348 0.047 Uiso 1 1 calc R . .
C33 C 0.2013(4) 0.5787(3) 0.4771(3) 0.0536(9) Uani 1 1 d . . .
H33 H 0.2167 0.6458 0.4519 0.064 Uiso 1 1 calc R . .
C34 C 0.1175(3) 0.4984(3) 0.4049(3) 0.0478(8) Uani 1 1 d . . .
H34 H 0.0742 0.5111 0.3321 0.057 Uiso 1 1 calc R . .
C35 C 0.0995(3) 0.3987(3) 0.4433(2) 0.0356(7) Uani 1 1 d . . .
C36 C 0.1633(2) 0.3821(2) 0.5522(2) 0.0262(6) Uani 1 1 d . . .
C37 C 0.0167(3) 0.2946(3) 0.3876(2) 0.0447(8) Uani 1 1 d . . .
H37 H 0.0310 0.2698 0.3218 0.054 Uiso 1 1 calc R . .
H371 H -0.0743 0.3060 0.3690 0.054 Uiso 1 1 calc R . .
C38 C 0.0628(3) 0.2118(2) 0.4743(2) 0.0365(7) Uani 1 1 d . . .
C39 C -0.0462(3) 0.1485(3) 0.4934(2) 0.0465(8) Uani 1 1 d . . .
H39 H -0.0107 0.0982 0.5484 0.070 Uiso 1 1 calc R . .
H391 H -0.1008 0.1075 0.4266 0.070 Uiso 1 1 calc R . .
H392 H -0.0959 0.1998 0.5173 0.070 Uiso 1 1 calc R . .
C310 C 0.1559(3) 0.1352(2) 0.4508(2) 0.0424(8) Uani 1 1 d . . .
H31A H 0.2221 0.1785 0.4380 0.064 Uiso 1 1 calc R . .
H31B H 0.1099 0.0857 0.3872 0.064 Uiso 1 1 calc R . .
H31C H 0.1947 0.0930 0.5123 0.064 Uiso 1 1 calc R . .
C41 C 0.3189(2) 0.6472(2) 0.9192(2) 0.0265(6) Uani 1 1 d . . .
H41 H 0.3324 0.6713 0.8553 0.032 Uiso 1 1 calc R . .
H411 H 0.3391 0.7103 0.9732 0.032 Uiso 1 1 calc R . .
C42 C 0.1809(2) 0.6066(2) 0.8884(2) 0.0341(7) Uani 1 1 d . . .
H42 H 0.1260 0.6652 0.8594 0.051 Uiso 1 1 calc R . .
H421 H 0.1673 0.5837 0.9519 0.051 Uiso 1 1 calc R . .
H422 H 0.1606 0.5448 0.8341 0.051 Uiso 1 1 calc R . .
C511 C 0.6630(12) 0.5580(11) 0.7945(9) 0.028(3) Uani 0.522(7) 1 d P A 1
H51A H 0.7140 0.4949 0.8183 0.034 Uiso 0.522(7) 1 calc PR A 1
H51B H 0.7202 0.6248 0.8189 0.034 Uiso 0.522(7) 1 calc PR A 1
C521 C 0.5991(6) 0.5477(5) 0.6694(5) 0.047(2) Uani 0.522(7) 1 d P A 1
H52A H 0.6647 0.5479 0.6384 0.070 Uiso 0.522(7) 1 calc PR A 1
H52B H 0.5466 0.6092 0.6463 0.070 Uiso 0.522(7) 1 calc PR A 1
H52C H 0.5460 0.4796 0.6453 0.070 Uiso 0.522(7) 1 calc PR A 1
C512 C 0.6231(15) 0.5655(14) 0.7616(11) 0.043(4) Uani 0.478(7) 1 d P A 2
H51C H 0.5912 0.6250 0.7151 0.052 Uiso 0.478(7) 1 calc PR A 2
H51D H 0.6039 0.4959 0.7162 0.052 Uiso 0.478(7) 1 calc PR A 2
C522 C 0.7673(7) 0.5849(6) 0.8246(6) 0.055(2) Uani 0.478(7) 1 d P A 2
H52D H 0.8118 0.5808 0.7745 0.082 Uiso 0.478(7) 1 calc PR A 2
H52E H 0.7960 0.5292 0.8751 0.082 Uiso 0.478(7) 1 calc PR A 2
H52F H 0.7856 0.6569 0.8640 0.082 Uiso 0.478(7) 1 calc PR A 2
HO51 H 0.571(4) 0.619(3) 0.871(3) 0.071(13) 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'
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
O31 Zr O11 97.11(7) . . ?
O31 Zr O21 100.38(7) . . ?
O11 Zr O21 99.13(7) . . ?
O31 Zr O41 95.66(6) . . ?
O11 Zr O41 160.08(6) . . ?
O21 Zr O41 93.53(7) . . ?
O31 Zr O41 166.46(6) . 2_667 ?
O11 Zr O41 92.59(6) . 2_667 ?
O21 Zr O41 87.32(7) . 2_667 ?
O41 Zr O41 72.59(7) . 2_667 ?
O31 Zr O51 88.03(7) . . ?
O11 Zr O51 86.86(7) . . ?
O21 Zr O51 168.91(7) . . ?
O41 Zr O51 78.35(7) . . ?
O41 Zr O51 83.07(7) 2_667 . ?
O31 Zr Zr 132.09(5) . 2_667 ?
O11 Zr Zr 127.24(5) . 2_667 ?
O21 Zr Zr 90.48(5) . 2_667 ?
O41 Zr Zr 36.76(4) . 2_667 ?
O41 Zr Zr 35.83(4) 2_667 2_667 ?
O51 Zr Zr 78.49(5) . 2_667 ?
C16 O10 C18 108.09(18) . . ?
C11 O11 Zr 160.80(15) . . ?
C26 O20 C28 106.40(18) . . ?
C21 O21 Zr 139.91(15) . . ?
C36 O30 C38 107.11(19) . . ?
C31 O31 Zr 160.79(15) . . ?
C41 O41 Zr 127.26(14) . . ?
C41 O41 Zr 122.91(13) . 2_667 ?
Zr O41 Zr 107.41(7) . 2_667 ?
C512 O51 C511 20.2(7) . . ?
C512 O51 Zr 129.5(7) . . ?
C511 O51 Zr 129.8(6) . . ?
O11 C11 C12 122.3(2) . . ?
O11 C11 C16 121.1(2) . . ?
C12 C11 C16 116.6(2) . . ?
C13 C12 C11 121.6(2) . . ?
C12 C13 C14 120.9(2) . . ?
C15 C14 C13 118.1(2) . . ?
C14 C15 C16 120.5(2) . . ?
C14 C15 C17 131.6(2) . . ?
C16 C15 C17 107.8(2) . . ?
O10 C16 C15 114.5(2) . . ?
O10 C16 C11 123.2(2) . . ?
C15 C16 C11 122.2(2) . . ?
C15 C17 C18 103.9(2) . . ?
O10 C18 C110 107.1(2) . . ?
O10 C18 C19 106.0(2) . . ?
C110 C18 C19 113.2(2) . . ?
O10 C18 C17 105.4(2) . . ?
C110 C18 C17 112.2(2) . . ?
C19 C18 C17 112.3(2) . . ?
O21 C21 C26 120.6(2) . . ?
O21 C21 C22 122.7(2) . . ?
C26 C21 C22 116.7(2) . . ?
C23 C22 C21 120.9(2) . . ?
C22 C23 C24 121.3(2) . . ?
C23 C24 C25 118.4(2) . . ?
C26 C25 C24 119.8(2) . . ?
C26 C25 C27 107.2(2) . . ?
C24 C25 C27 132.9(2) . . ?
C25 C26 O20 114.1(2) . . ?
C25 C26 C21 122.7(2) . . ?
O20 C26 C21 123.2(2) . . ?
C25 C27 C28 102.6(2) . . ?
O20 C28 C29 107.4(2) . . ?
O20 C28 C210 107.2(2) . . ?
C29 C28 C210 112.3(2) . . ?
O20 C28 C27 103.67(19) . . ?
C29 C28 C27 114.6(2) . . ?
C210 C28 C27 110.9(2) . . ?
O31 C31 C32 122.6(2) . . ?
O31 C31 C36 121.3(2) . . ?
C32 C31 C36 116.1(2) . . ?
C31 C32 C33 120.8(3) . . ?
C34 C33 C32 121.8(3) . . ?
C33 C34 C35 118.0(3) . . ?
C34 C35 C36 120.1(3) . . ?
C34 C35 C37 131.8(3) . . ?
C36 C35 C37 108.1(2) . . ?
O30 C36 C35 113.4(2) . . ?
O30 C36 C31 123.4(2) . . ?
C35 C36 C31 123.1(3) . . ?
C35 C37 C38 102.7(2) . . ?
O30 C38 C39 105.9(2) . . ?
O30 C38 C310 107.2(2) . . ?
C39 C38 C310 112.3(3) . . ?
O30 C38 C37 106.0(2) . . ?
C39 C38 C37 113.8(3) . . ?
C310 C38 C37 111.2(2) . . ?
O41 C41 C42 110.6(2) . . ?
O51 C511 C521 109.8(8) . . ?
O51 C512 C522 106.5(8) . . ?
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 O31 1.9637(16) . ?
Zr O11 1.9685(15) . ?
Zr O21 2.0086(16) . ?
Zr O41 2.1310(15) . ?
Zr O41 2.1785(16) 2_667 ?
Zr O51 2.2774(19) . ?
Zr Zr 3.4734(5) 2_667 ?
O10 C16 1.367(3) . ?
O10 C18 1.488(3) . ?
O11 C11 1.354(3) . ?
O20 C26 1.384(3) . ?
O20 C28 1.495(3) . ?
O21 C21 1.346(3) . ?
O30 C36 1.373(3) . ?
O30 C38 1.479(3) . ?
O31 C31 1.360(3) . ?
O41 C41 1.454(3) . ?
O41 Zr 2.1785(16) 2_667 ?
O51 C512 1.453(18) . ?
O51 C511 1.467(15) . ?
C11 C12 1.389(3) . ?
C11 C16 1.391(3) . ?
C12 C13 1.386(3) . ?
C13 C14 1.393(4) . ?
C14 C15 1.379(3) . ?
C15 C16 1.387(3) . ?
C15 C17 1.505(4) . ?
C17 C18 1.557(4) . ?
C18 C110 1.494(4) . ?
C18 C19 1.501(4) . ?
C21 C26 1.394(3) . ?
C21 C22 1.394(3) . ?
C22 C23 1.385(4) . ?
C23 C24 1.386(4) . ?
C24 C25 1.389(3) . ?
C25 C26 1.375(3) . ?
C25 C27 1.509(3) . ?
C27 C28 1.551(4) . ?
C28 C29 1.502(4) . ?
C28 C210 1.521(3) . ?
C31 C32 1.387(4) . ?
C31 C36 1.390(3) . ?
C32 C33 1.400(4) . ?
C33 C34 1.372(5) . ?
C34 C35 1.376(4) . ?
C35 C36 1.383(3) . ?
C35 C37 1.508(4) . ?
C37 C38 1.530(4) . ?
C38 C39 1.518(4) . ?
C38 C310 1.518(4) . ?
C41 C42 1.495(3) . ?
C511 C521 1.534(11) . ?
C512 C522 1.516(15) . ?
