#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:32:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179145 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/06/4310606.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_4310606
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 N8 O14 Zr2'
_chemical_formula_weight         1429.65
_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                104.260(10)
_cell_angle_beta                 104.240(10)
_cell_angle_gamma                107.200(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0480(10)
_cell_length_b                   12.4910(10)
_cell_length_c                   13.0520(10)
_cell_measurement_temperature    153(2)
_cell_volume                     1707.3(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1198
_diffrn_reflns_av_sigmaI/netI    0.3122
_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       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8552
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.02
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.525
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         8198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.2783
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.884
_refine_ls_shift/su_mean         0.116
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0966P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2776
_reflns_number_gt                3454
_reflns_number_total             8198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035067csi20031204_123245_2.cif
_cod_data_source_block           7
_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 
;
_cod_original_cell_volume        1707.3(2)
_cod_database_code               4310606
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
Zr1 Zr 0.61094(10) 0.52334(9) 0.62913(8) 0.0231(3) Uani 1 1 d . . .
Cl1 Cl 0.7343(3) 0.7408(2) 0.7082(2) 0.0412(8) Uani 1 1 d . . .
Cl2 Cl 0.7444(3) 0.4405(3) 0.5500(2) 0.0414(7) Uani 1 1 d . . .
O1 O 0.5222(6) 0.5573(6) 0.7448(5) 0.0286(17) Uani 1 1 d . . .
O2 O 0.4707(7) 0.5692(7) 0.8991(6) 0.041(2) Uani 1 1 d . . .
O3 O 0.4294(7) 0.4277(6) 0.5162(5) 0.0290(17) Uani 1 1 d . . .
H3 H 0.362(9) 0.378(9) 0.527(8) 0.035 Uiso 1 1 d . . .
N1 N 0.7623(8) 0.5469(7) 0.8026(7) 0.029(2) Uani 1 1 d . . .
N2 N 0.7210(8) 0.5108(7) 0.8828(6) 0.026(2) Uani 1 1 d . . .
N3 N 0.5457(7) 0.3404(7) 0.6646(6) 0.0257(19) Uani 1 1 d . . .
N4 N 0.5407(8) 0.3405(7) 0.7675(6) 0.026(2) Uani 1 1 d . . .
C1 C 0.5911(9) 0.4537(8) 0.8606(8) 0.023(2) Uani 1 1 d . . .
H1 H 0.5806 0.4367 0.9278 0.027 Uiso 1 1 calc R . .
C2 C 0.5212(9) 0.5334(9) 0.8357(7) 0.023(2) Uani 1 1 d . . .
C3 C 0.8849(9) 0.5926(10) 0.8459(8) 0.030(2) Uani 1 1 d . . .
C4 C 0.9226(9) 0.5847(8) 0.9520(8) 0.025(2) Uani 1 1 d . . .
H4 H 1.0041 0.6098 0.9990 0.030 Uiso 1 1 calc R . .
C5 C 0.8199(10) 0.5339(9) 0.9754(8) 0.027(2) Uani 1 1 d . . .
C6 C 0.9691(10) 0.6419(11) 0.7875(9) 0.042(3) Uani 1 1 d . . .
H6A H 0.9700 0.5775 0.7300 0.050 Uiso 1 1 calc R . .
H6B H 1.0513 0.6867 0.8411 0.050 Uiso 1 1 calc R . .
H6C H 0.9402 0.6933 0.7539 0.050 Uiso 1 1 calc R . .
C7 C 0.8040(10) 0.5015(11) 1.0737(9) 0.040(3) Uani 1 1 d . . .
H7A H 0.7518 0.5369 1.1017 0.048 Uiso 1 1 calc R . .
H7B H 0.8833 0.5303 1.1317 0.048 Uiso 1 1 calc R . .
H7C H 0.7665 0.4163 1.0517 0.048 Uiso 1 1 calc R . .
C8 C 0.5000(9) 0.2247(8) 0.6002(8) 0.026(2) Uani 1 1 d . . .
C9 C 0.4662(10) 0.1542(9) 0.6651(9) 0.032(3) Uani 1 1 d . . .
H9 H 0.4311 0.0713 0.6401 0.039 Uiso 1 1 calc R . .
C10 C 0.4940(10) 0.2286(9) 0.7696(9) 0.030(2) Uani 1 1 d . . .
C11 C 0.4898(11) 0.1828(9) 0.4805(8) 0.041(3) Uani 1 1 d . . .
H11A H 0.4448 0.2200 0.4397 0.050 Uiso 1 1 calc R . .
H11B H 0.4468 0.0977 0.4487 0.050 Uiso 1 1 calc R . .
H11C H 0.5711 0.2036 0.4754 0.050 Uiso 1 1 calc R . .
C12 C 0.4815(13) 0.2032(11) 0.8747(10) 0.053(4) Uani 1 1 d . . .
H12A H 0.4269 0.2372 0.8997 0.063 Uiso 1 1 calc R . .
H12B H 0.5614 0.2379 0.9329 0.063 Uiso 1 1 calc R . .
H12C H 0.4484 0.1185 0.8583 0.063 Uiso 1 1 calc R . .
O20 O 0.885(2) 0.9221(18) 1.2104(15) 0.188(8) Uani 1 1 d . . .
C20 C 0.8326(18) 0.8133(13) 1.1303(12) 0.076(5) Uani 1 1 d . . .
H20A H 0.7586 0.7667 1.1405 0.091 Uiso 1 1 calc R . .
H20B H 0.8894 0.7721 1.1366 0.091 Uiso 1 1 calc R . .
C21 C 0.8015(18) 0.8242(15) 1.0225(13) 0.090(6) Uani 1 1 d . . .
H21A H 0.7156 0.7743 0.9784 0.108 Uiso 1 1 calc R . .
H21B H 0.8531 0.7998 0.9827 0.108 Uiso 1 1 calc R . .
C22 C 0.822(2) 0.949(2) 1.0399(19) 0.133(8) Uani 1 1 d . . .
H22A H 0.8550 0.9744 0.9854 0.160 Uiso 1 1 calc R . .
H22B H 0.7462 0.9626 1.0346 0.160 Uiso 1 1 calc R . .
C23 C 0.911(2) 1.0097(17) 1.1523(19) 0.131(9) Uani 1 1 d . . .
H23A H 0.9003 1.0815 1.1891 0.157 Uiso 1 1 calc R . .
H23B H 0.9950 1.0313 1.1511 0.157 Uiso 1 1 calc R . .
O30 O 0.7882(8) 0.2632(7) 0.8631(7) 0.050(2) Uani 1 1 d . . .
C30 C 0.7833(15) 0.1529(12) 0.8772(12) 0.069(4) Uani 1 1 d . . .
H30A H 0.7199 0.1253 0.9088 0.083 Uiso 1 1 calc R . .
H30B H 0.8622 0.1626 0.9280 0.083 Uiso 1 1 calc R . .
C31 C 0.755(2) 0.0689(14) 0.7696(14) 0.108(7) Uani 1 1 d . . .
H31A H 0.6685 0.0170 0.7399 0.130 Uiso 1 1 calc R . .
H31B H 0.8043 0.0200 0.7759 0.130 Uiso 1 1 calc R . .
C32 C 0.7846(15) 0.1362(13) 0.6916(12) 0.076(5) Uani 1 1 d . . .
H32A H 0.8537 0.1264 0.6706 0.091 Uiso 1 1 calc R . .
H32B H 0.7134 0.1103 0.6241 0.091 Uiso 1 1 calc R . .
C33 C 0.8171(12) 0.2632(11) 0.7632(10) 0.050(3) Uani 1 1 d . . .
H33A H 0.9045 0.3089 0.7828 0.060 Uiso 1 1 calc R . .
H33B H 0.7703 0.2997 0.7218 0.060 Uiso 1 1 calc R . .
O40 O 0.2554(8) 0.2931(8) 0.5799(7) 0.054(2) Uani 1 1 d . . .
C41 C 0.0452(16) 0.1863(18) 0.4998(15) 0.108(7) Uani 1 1 d . . .
H41A H 0.0065 0.1764 0.4218 0.130 Uiso 1 1 calc R . .
H41B H -0.0087 0.1254 0.5186 0.130 Uiso 1 1 calc R . .
C42 C 0.0669(17) 0.3041(18) 0.573(2) 0.138(10) Uani 1 1 d . . .
H42A H 0.0400 0.3498 0.5287 0.166 Uiso 1 1 calc R . .
H42B H 0.0219 0.2982 0.6247 0.166 Uiso 1 1 calc R . .
C43 C 0.1969(15) 0.3599(14) 0.6327(13) 0.081(5) Uani 1 1 d . . .
H43A H 0.2276 0.4409 0.6324 0.098 Uiso 1 1 calc R . .
H43B H 0.2143 0.3631 0.7102 0.098 Uiso 1 1 calc R . .
O50 O 0.5910(13) 0.0890(10) 0.2621(11) 0.100(4) Uani 1 1 d . . .
C50 C 0.7104(18) 0.154(2) 0.3155(19) 0.112(7) Uani 1 1 d . . .
H50A H 0.7568 0.1028 0.3043 0.134 Uiso 1 1 calc R . .
H50B H 0.7256 0.1847 0.3956 0.134 Uiso 1 1 calc R . .
C51 C 0.751(2) 0.246(2) 0.279(2) 0.159(12) Uani 1 1 d . . .
H51A H 0.8205 0.2425 0.2546 0.191 Uiso 1 1 calc R . .
H51B H 0.7787 0.3216 0.3394 0.191 Uiso 1 1 calc R . .
C52 C 0.653(3) 0.235(3) 0.190(3) 0.195(16) Uani 1 1 d . . .
H52A H 0.6678 0.2108 0.1196 0.233 Uiso 1 1 calc R . .
H52B H 0.6434 0.3110 0.1999 0.233 Uiso 1 1 calc R . .
C53 C 0.5442(19) 0.149(2) 0.1856(18) 0.122(8) Uani 1 1 d . . .
H53A H 0.4981 0.0925 0.1097 0.147 Uiso 1 1 calc R . .
H53B H 0.4916 0.1860 0.2122 0.147 Uiso 1 1 calc R . .
C40 C 0.1645(14) 0.1766(12) 0.5171(13) 0.070(4) Uani 1 1 d . . .
H40A H 0.1724 0.1227 0.5582 0.084 Uiso 1 1 calc R . .
H40B H 0.1742 0.1461 0.4453 0.084 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'
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 Zr1 O3 83.1(3) . . ?
O1 Zr1 O3 119.5(3) . 2_666 ?
O3 Zr1 O3 65.8(3) . 2_666 ?
O1 Zr1 N3 76.5(3) . . ?
O3 Zr1 N3 75.1(3) . . ?
O3 Zr1 N3 134.2(3) 2_666 . ?
O1 Zr1 N1 78.2(3) . . ?
O3 Zr1 N1 145.8(3) . . ?
O3 Zr1 N1 148.3(3) 2_666 . ?
N3 Zr1 N1 72.8(3) . . ?
O1 Zr1 Cl2 154.82(18) . . ?
O3 Zr1 Cl2 107.1(2) . . ?
O3 Zr1 Cl2 85.5(2) 2_666 . ?
N3 Zr1 Cl2 83.9(2) . . ?
N1 Zr1 Cl2 81.0(2) . . ?
O1 Zr1 Cl1 85.6(2) . . ?
O3 Zr1 Cl1 130.3(2) . . ?
O3 Zr1 Cl1 78.7(2) 2_666 . ?
N3 Zr1 Cl1 147.1(2) . . ?
N1 Zr1 Cl1 76.8(2) . . ?
Cl2 Zr1 Cl1 103.35(11) . . ?
O1 Zr1 Zr1 102.94(18) . 2_666 ?
O3 Zr1 Zr1 33.14(18) . 2_666 ?
O3 Zr1 Zr1 32.7(2) 2_666 2_666 ?
N3 Zr1 Zr1 105.42(18) . 2_666 ?
N1 Zr1 Zr1 177.6(2) . 2_666 ?
Cl2 Zr1 Zr1 97.33(8) . 2_666 ?
Cl1 Zr1 Zr1 105.33(8) . 2_666 ?
C2 O1 Zr1 134.4(6) . . ?
Zr1 O3 Zr1 114.2(3) . 2_666 ?
C3 N1 N2 106.4(8) . . ?
C3 N1 Zr1 134.9(7) . . ?
N2 N1 Zr1 118.7(6) . . ?
C5 N2 N1 109.9(8) . . ?
C5 N2 C1 129.6(8) . . ?
N1 N2 C1 120.4(8) . . ?
C8 N3 N4 105.0(8) . . ?
C8 N3 Zr1 134.2(6) . . ?
N4 N3 Zr1 120.6(6) . . ?
C10 N4 N3 112.2(8) . . ?
C10 N4 C1 128.4(8) . . ?
N3 N4 C1 119.3(8) . . ?
N2 C1 N4 109.6(8) . . ?
N2 C1 C2 111.8(8) . . ?
N4 C1 C2 110.8(7) . . ?
O2 C2 O1 125.4(9) . . ?
O2 C2 C1 120.2(8) . . ?
O1 C2 C1 114.4(8) . . ?
N1 C3 C4 109.6(9) . . ?
N1 C3 C6 125.1(9) . . ?
C4 C3 C6 125.3(9) . . ?
C5 C4 C3 108.1(8) . . ?
C4 C5 N2 106.0(8) . . ?
C4 C5 C7 131.9(9) . . ?
N2 C5 C7 122.0(10) . . ?
N3 C8 C9 109.1(9) . . ?
N3 C8 C11 123.4(9) . . ?
C9 C8 C11 127.5(9) . . ?
C10 C9 C8 107.5(9) . . ?
C9 C10 N4 106.2(9) . . ?
C9 C10 C12 130.8(10) . . ?
N4 C10 C12 123.0(9) . . ?
C20 O20 C23 106.8(15) . . ?
O20 C20 C21 109.8(13) . . ?
C20 C21 C22 107.0(14) . . ?
C23 C22 C21 103.3(16) . . ?
C22 C23 O20 104.3(16) . . ?
C30 O30 C33 107.1(10) . . ?
O30 C30 C31 107.8(12) . . ?
C30 C31 C32 108.7(13) . . ?
C33 C32 C31 102.2(12) . . ?
O30 C33 C32 108.7(11) . . ?
C43 O40 C40 107.0(11) . . ?
C42 C41 C40 106.9(15) . . ?
C43 C42 C41 106.2(16) . . ?
O40 C43 C42 108.5(14) . . ?
C50 O50 C53 106.7(15) . . ?
O50 C50 C51 112(2) . . ?
C50 C51 C52 106.9(19) . . ?
C51 C52 C53 108.9(18) . . ?
C52 C53 O50 103.5(15) . . ?
O40 C40 C41 106.8(13) . . ?
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
Zr1 O1 2.085(7) . ?
Zr1 O3 2.094(7) . ?
Zr1 O3 2.121(6) 2_666 ?
Zr1 N3 2.386(8) . ?
Zr1 N1 2.421(8) . ?
Zr1 Cl2 2.449(3) . ?
Zr1 Cl1 2.476(3) . ?
Zr1 Zr1 3.539(2) 2_666 ?
O1 C2 1.294(10) . ?
O2 C2 1.218(11) . ?
O3 Zr1 2.121(6) 2_666 ?
N1 C3 1.326(12) . ?
N1 N2 1.379(10) . ?
N2 C5 1.371(11) . ?
N2 C1 1.435(12) . ?
N3 C8 1.342(12) . ?
N3 N4 1.359(10) . ?
N4 C10 1.353(12) . ?
N4 C1 1.459(11) . ?
C1 C2 1.525(13) . ?
C3 C4 1.385(13) . ?
C3 C6 1.494(14) . ?
C4 C5 1.358(14) . ?
C5 C7 1.476(14) . ?
C8 C9 1.407(14) . ?
C8 C11 1.482(13) . ?
C9 C10 1.343(14) . ?
C10 C12 1.514(14) . ?
O20 C20 1.34(2) . ?
O20 C23 1.48(2) . ?
C20 C21 1.416(19) . ?
C21 C22 1.45(2) . ?
C22 C23 1.44(3) . ?
O30 C30 1.420(14) . ?
O30 C33 1.431(14) . ?
C30 C31 1.421(19) . ?
C31 C32 1.51(2) . ?
C32 C33 1.505(17) . ?
O40 C43 1.403(16) . ?
O40 C40 1.421(15) . ?
C41 C42 1.45(2) . ?
C41 C40 1.44(2) . ?
C42 C43 1.43(2) . ?
O50 C50 1.323(19) . ?
O50 C53 1.49(2) . ?
C50 C51 1.36(3) . ?
C51 C52 1.39(3) . ?
C52 C53 1.40(3) . ?
