#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:32:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179145 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/06/4310607.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_4310607
loop_
_publ_author_name
'A. Otero'
'J. Fernández-Baeza'
'A. Antiñolo'
'J. Tejeda'
'A. Lara-Sánchez'
'L. Sánchez-Barba'
'M. Fernández-López'
'I. López-Solera'
_publ_contact_author
;
Isabel López-Solera
Departamento de Química Inórganica, Orgánica y Bioquímica
Facultad de Químicas
Universidad Castilla La Mancha
13071-Ciudad Real 
Spain
;
_publ_contact_author_email       Mabel.Lopez@uclm.es
_publ_contact_author_fax         '+34 926 295318'
_publ_contact_author_phone       '+34 926 295300 (ext:3477)'
_publ_section_title
;
 New Complexes of Zirconium(IV) and Hafnium(IV) with Heteroscorpionate
 Ligands and the Hydrolysis of Such Complexes To Give a Zirconium Cluster#
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1350
_journal_page_last               1358
_journal_paper_doi               10.1021/ic035067c
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C56 H96 Cl4 Hf2 N8 O14'
_chemical_formula_weight         1604.19
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.24(10)
_cell_angle_beta                 104.05(10)
_cell_angle_gamma                107.16(10)
_cell_formula_units_Z            1
_cell_length_a                   11.9860(10)
_cell_length_b                   12.4780(10)
_cell_length_c                   12.9700(10)
_cell_measurement_temperature    153(2)
_cell_volume                     1689(2)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7894
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        36
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.293
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.280
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.014
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.084
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0531P)²+0.6105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                6501
_reflns_number_total             7543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035067csi20031204_123245_3.cif
_cod_data_source_block           8
_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_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1689.2(2)
_cod_database_code               4310607
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
Hf1 Hf 0.610716(16) 0.522743(14) 0.628862(15) 0.02558(7) Uani 1 1 d . . .
Cl1 Cl 0.73329(11) 0.73962(9) 0.70769(11) 0.0419(3) Uani 1 1 d . . .
Cl2 Cl 0.74229(12) 0.44086(11) 0.54862(11) 0.0422(3) Uani 1 1 d . . .
O1 O 0.5218(3) 0.5582(3) 0.7443(3) 0.0296(6) Uani 1 1 d . . .
O2 O 0.4703(3) 0.5691(3) 0.8987(3) 0.0395(8) Uani 1 1 d . . .
O3 O 0.4302(3) 0.4269(3) 0.5150(3) 0.0322(7) Uani 1 1 d . . .
H3 H 0.380(5) 0.383(4) 0.531(4) 0.028(13) Uiso 1 1 d . . .
N1 N 0.7599(3) 0.5450(3) 0.8004(3) 0.0276(7) Uani 1 1 d . . .
N2 N 0.7221(3) 0.5118(3) 0.8828(3) 0.0265(7) Uani 1 1 d . . .
N3 N 0.5468(3) 0.3413(3) 0.6645(3) 0.0265(7) Uani 1 1 d . . .
N4 N 0.5403(3) 0.3409(3) 0.7674(3) 0.0277(8) Uani 1 1 d . . .
C1 C 0.5910(4) 0.4537(4) 0.8608(4) 0.0270(9) Uani 1 1 d . . .
H1 H 0.5802 0.4372 0.9286 0.032 Uiso 1 1 calc R . .
C2 C 0.5203(4) 0.5347(4) 0.8343(4) 0.0298(9) Uani 1 1 d . . .
C3 C 0.8843(4) 0.5908(4) 0.8442(4) 0.0314(9) Uani 1 1 d . . .
C4 C 0.9226(4) 0.5852(4) 0.9521(4) 0.0320(10) Uani 1 1 d . . .
H4 H 1.0041 0.6119 1.0002 0.038 Uiso 1 1 calc R . .
C5 C 0.8183(4) 0.5332(4) 0.9741(4) 0.0289(9) Uani 1 1 d . . .
C6 C 0.9668(4) 0.6383(5) 0.7842(5) 0.0444(12) Uani 1 1 d . . .
H6A H 0.9645 0.5734 0.7247 0.053 Uiso 1 1 calc R . .
H6B H 1.0502 0.6804 0.8365 0.053 Uiso 1 1 calc R . .
H6C H 0.9392 0.6917 0.7526 0.053 Uiso 1 1 calc R . .
C7 C 0.8027(5) 0.5010(5) 1.0731(4) 0.0436(12) Uani 1 1 d . . .
H7A H 0.7419 0.5276 1.0954 0.052 Uiso 1 1 calc R . .
H7B H 0.8805 0.5387 1.1345 0.052 Uiso 1 1 calc R . .
H7C H 0.7754 0.4160 1.0539 0.052 Uiso 1 1 calc R . .
C8 C 0.4947(4) 0.2300(4) 0.7702(4) 0.0363(10) Uani 1 1 d . . .
C9 C 0.4671(4) 0.1546(4) 0.6629(4) 0.0383(11) Uani 1 1 d . . .
H9 H 0.4322 0.0716 0.6372 0.046 Uiso 1 1 calc R . .
C10 C 0.5014(4) 0.2258(4) 0.6002(4) 0.0326(10) Uani 1 1 d . . .
C11 C 0.4831(6) 0.2060(5) 0.8734(5) 0.0524(14) Uani 1 1 d . . .
H11A H 0.5639 0.2375 0.9302 0.063 Uiso 1 1 calc R . .
H11B H 0.4463 0.1214 0.8566 0.063 Uiso 1 1 calc R . .
H11C H 0.4315 0.2435 0.9007 0.063 Uiso 1 1 calc R . .
C12 C 0.4901(5) 0.1834(4) 0.4787(4) 0.0432(12) Uani 1 1 d . . .
H12A H 0.4147 0.1843 0.4327 0.052 Uiso 1 1 calc R . .
H12B H 0.4887 0.1035 0.4578 0.052 Uiso 1 1 calc R . .
H12C H 0.5598 0.2351 0.4675 0.052 Uiso 1 1 calc R . .
O20 O 0.7885(4) 0.2632(3) 0.8635(4) 0.0517(10) Uani 1 1 d . . .
C20 C 0.7856(8) 0.1547(6) 0.8783(7) 0.072(2) Uani 1 1 d . . .
H20A H 0.7241 0.1279 0.9126 0.087 Uiso 1 1 calc R . .
H20B H 0.8660 0.1651 0.9277 0.087 Uiso 1 1 calc R . .
C21 C 0.7550(12) 0.0687(7) 0.7704(7) 0.113(4) Uani 1 1 d . . .
H21A H 0.6678 0.0173 0.7422 0.136 Uiso 1 1 calc R . .
H21B H 0.8042 0.0197 0.7757 0.136 Uiso 1 1 calc R . .
C22 C 0.7826(7) 0.1365(6) 0.6924(6) 0.0688(19) Uani 1 1 d . . .
H22A H 0.7104 0.1108 0.6254 0.083 Uiso 1 1 calc R . .
H22B H 0.8512 0.1262 0.6695 0.083 Uiso 1 1 calc R . .
C23 C 0.8163(6) 0.2637(5) 0.7634(6) 0.0559(15) Uani 1 1 d . . .
H23A H 0.9040 0.3088 0.7821 0.067 Uiso 1 1 calc R . .
H23B H 0.7691 0.3004 0.7223 0.067 Uiso 1 1 calc R . .
O30 O 0.2575(4) 0.2924(4) 0.5799(4) 0.0572(11) Uani 1 1 d . . .
C30 C 0.1664(6) 0.1753(6) 0.5172(7) 0.0680(19) Uani 1 1 d . . .
H30A H 0.1767 0.1209 0.5574 0.082 Uiso 1 1 calc R . .
H30B H 0.1741 0.1460 0.4437 0.082 Uiso 1 1 calc R . .
C31 C 0.0461(7) 0.1841(9) 0.5041(9) 0.120(4) Uani 1 1 d . . .
H31A H -0.0032 0.1270 0.5303 0.145 Uiso 1 1 calc R . .
H31B H 0.0016 0.1676 0.4251 0.145 Uiso 1 1 calc R . .
C32 C 0.0681(8) 0.3043(9) 0.5707(12) 0.137(5) Uani 1 1 d . . .
H32A H 0.0213 0.3032 0.6222 0.164 Uiso 1 1 calc R . .
H32B H 0.0433 0.3472 0.5221 0.164 Uiso 1 1 calc R . .
C33 C 0.2007(7) 0.3607(7) 0.6336(7) 0.087(3) Uani 1 1 d . . .
H33A H 0.2327 0.4418 0.6336 0.104 Uiso 1 1 calc R . .
H33B H 0.2169 0.3632 0.7113 0.104 Uiso 1 1 calc R . .
O40 O 1.1685(8) 1.1855(7) 0.8671(7) 0.123(3) Uani 1 1 d . . .
C40 C 1.1148(11) 1.0714(9) 0.7897(8) 0.110(3) Uani 1 1 d . . .
H40A H 1.1718 1.0559 0.7517 0.132 Uiso 1 1 calc R . .
H40B H 1.0399 1.0630 0.7332 0.132 Uiso 1 1 calc R . .
C41 C 1.0855(12) 0.9890(8) 0.8455(11) 0.141(5) Uani 1 1 d . . .
H41A H 1.0969 0.9165 0.8111 0.169 Uiso 1 1 calc R . .
H41B H 1.0006 0.9688 0.8446 0.169 Uiso 1 1 calc R . .
C42 C 1.1762(13) 1.0551(9) 0.9635(10) 0.131(4) Uani 1 1 d . . .
H42A H 1.1406 1.0324 1.0182 0.158 Uiso 1 1 calc R . .
H42B H 1.2517 1.0391 0.9718 0.158 Uiso 1 1 calc R . .
C43 C 1.2005(9) 1.1765(6) 0.9779(7) 0.081(2) Uani 1 1 d . . .
H43A H 1.2876 1.2244 1.0205 0.097 Uiso 1 1 calc R . .
H43B H 1.1511 1.2050 1.0188 0.097 Uiso 1 1 calc R . .
O50 O 0.5927(6) 0.0898(4) 0.2623(5) 0.0941(18) Uani 1 1 d . . .
C50 C 0.7141(9) 0.1561(11) 0.3181(10) 0.116(4) Uani 1 1 d . . .
H50A H 0.7634 0.1086 0.3036 0.139 Uiso 1 1 calc R . .
H50B H 0.7299 0.1847 0.3988 0.139 Uiso 1 1 calc R . .
C51 C 0.7459(15) 0.2528(12) 0.2797(11) 0.190(10) Uani 1 1 d . . .
H51A H 0.7566 0.3257 0.3363 0.228 Uiso 1 1 calc R . .
H51B H 0.8229 0.2634 0.2642 0.228 Uiso 1 1 calc R . .
C52 C 0.6511(16) 0.2272(16) 0.1833(15) 0.180(7) Uani 1 1 d . . .
H52A H 0.6684 0.1897 0.1173 0.216 Uiso 1 1 calc R . .
H52B H 0.6397 0.2995 0.1773 0.216 Uiso 1 1 calc R . .
C53 C 0.5447(9) 0.1491(11) 0.1910(10) 0.115(4) Uani 1 1 d . . .
H53A H 0.4895 0.0924 0.1170 0.138 Uiso 1 1 calc R . .
H53B H 0.5001 0.1927 0.2248 0.138 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 '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 Hf1 O3 83.64(13) . . ?
O1 Hf1 O3 118.21(13) . 2_666 ?
O3 Hf1 O3 65.56(15) . 2_666 ?
O1 Hf1 N3 77.33(12) . . ?
O3 Hf1 N3 75.31(12) . . ?
O3 Hf1 N3 134.65(12) 2_666 . ?
O1 Hf1 N1 78.53(12) . . ?
O3 Hf1 N1 145.76(12) . . ?
O3 Hf1 N1 148.57(12) 2_666 . ?
N3 Hf1 N1 72.39(12) . . ?
O1 Hf1 Cl2 155.83(9) . . ?
O3 Hf1 Cl2 106.23(10) . . ?
O3 Hf1 Cl2 85.84(10) 2_666 . ?
N3 Hf1 Cl2 83.85(9) . . ?
N1 Hf1 Cl2 81.43(9) . . ?
O1 Hf1 Cl1 85.01(9) . . ?
O3 Hf1 Cl1 130.37(9) . . ?
O3 Hf1 Cl1 78.20(9) 2_666 . ?
N3 Hf1 Cl1 147.11(9) . . ?
N1 Hf1 Cl1 77.07(9) . . ?
Cl2 Hf1 Cl1 103.57(5) . . ?
O1 Hf1 Hf1 102.53(8) . 2_666 ?
O3 Hf1 Hf1 32.97(9) . 2_666 ?
O3 Hf1 Hf1 32.59(9) 2_666 2_666 ?
N3 Hf1 Hf1 105.66(8) . 2_666 ?
N1 Hf1 Hf1 177.59(8) . 2_666 ?
Cl2 Hf1 Hf1 97.01(3) . 2_666 ?
Cl1 Hf1 Hf1 105.13(3) . 2_666 ?
C2 O1 Hf1 134.0(3) . . ?
Hf1 O3 Hf1 114.44(15) . 2_666 ?
C3 N1 N2 104.7(3) . . ?
C3 N1 Hf1 134.9(3) . . ?
N2 N1 Hf1 120.3(2) . . ?
C5 N2 N1 112.2(3) . . ?
C5 N2 C1 128.7(4) . . ?
N1 N2 C1 119.0(3) . . ?
C10 N3 N4 104.8(4) . . ?
C10 N3 Hf1 134.3(3) . . ?
N4 N3 Hf1 120.6(2) . . ?
C8 N4 N3 112.5(4) . . ?
C8 N4 C1 128.2(4) . . ?
N3 N4 C1 119.1(3) . . ?
N2 C1 N4 110.1(3) . . ?
N2 C1 C2 111.1(3) . . ?
N4 C1 C2 110.2(3) . . ?
O2 C2 O1 126.7(4) . . ?
O2 C2 C1 118.5(4) . . ?
O1 C2 C1 114.8(4) . . ?
N1 C3 C4 109.9(4) . . ?
N1 C3 C6 124.2(4) . . ?
C4 C3 C6 125.8(4) . . ?
C5 C4 C3 107.1(4) . . ?
N2 C5 C4 106.1(4) . . ?
N2 C5 C7 122.9(4) . . ?
C4 C5 C7 130.9(4) . . ?
N4 C8 C9 105.8(4) . . ?
N4 C8 C11 122.8(4) . . ?
C9 C8 C11 131.4(4) . . ?
C8 C9 C10 106.8(4) . . ?
N3 C10 C9 110.1(4) . . ?
N3 C10 C12 123.5(4) . . ?
C9 C10 C12 126.3(4) . . ?
C20 O20 C23 107.3(5) . . ?
O20 C20 C21 108.3(6) . . ?
C20 C21 C22 107.1(6) . . ?
C21 C22 C23 103.2(6) . . ?
O20 C23 C22 107.8(5) . . ?
C33 O30 C30 108.0(5) . . ?
O30 C30 C31 106.8(6) . . ?
C30 C31 C32 107.2(6) . . ?
C31 C32 C33 106.2(8) . . ?
O30 C33 C32 107.1(7) . . ?
C40 O40 C43 107.6(7) . . ?
O40 C40 C41 109.6(9) . . ?
C40 C41 C42 102.9(8) . . ?
C43 C42 C41 104.5(9) . . ?
C42 C43 O40 107.2(7) . . ?
C50 O50 C53 107.7(8) . . ?
O50 C50 C51 107.8(10) . . ?
C52 C51 C50 106.9(11) . . ?
C51 C52 C53 106.4(10) . . ?
C52 C53 O50 103.8(9) . . ?
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
Hf1 O1 2.074(3) . ?
Hf1 O3 2.084(3) . ?
Hf1 O3 2.106(3) 2_666 ?
Hf1 N3 2.364(3) . ?
Hf1 N1 2.387(4) . ?
Hf1 Cl2 2.4163(12) . ?
Hf1 Cl1 2.4679(11) . ?
Hf1 Hf1 3.5228(4) 2_666 ?
O1 C2 1.275(6) . ?
O2 C2 1.209(5) . ?
O3 Hf1 2.106(3) 2_666 ?
N1 C3 1.341(5) . ?
N1 N2 1.363(5) . ?
N2 C5 1.343(5) . ?
N2 C1 1.444(5) . ?
N3 C10 1.339(5) . ?
N3 N4 1.357(5) . ?
N4 C8 1.342(6) . ?
N4 C1 1.455(5) . ?
C1 C2 1.546(6) . ?
C3 C4 1.389(7) . ?
C3 C6 1.479(7) . ?
C4 C5 1.361(6) . ?
C5 C7 1.473(7) . ?
C8 C9 1.371(7) . ?
C8 C11 1.471(7) . ?
C9 C10 1.386(7) . ?
C10 C12 1.492(7) . ?
O20 C20 1.406(7) . ?
O20 C23 1.418(8) . ?
C20 C21 1.423(10) . ?
C21 C22 1.505(11) . ?
C22 C23 1.501(8) . ?
O30 C33 1.397(8) . ?
O30 C30 1.426(7) . ?
C30 C31 1.451(11) . ?
C31 C32 1.443(13) . ?
C32 C33 1.454(11) . ?
O40 C40 1.375(11) . ?
O40 C43 1.435(10) . ?
C40 C41 1.408(14) . ?
C41 C42 1.499(16) . ?
C42 C43 1.411(11) . ?
O50 C50 1.345(11) . ?
O50 C53 1.436(11) . ?
C50 C51 1.402(17) . ?
C51 C52 1.36(2) . ?
C52 C53 1.401(16) . ?
