New Complexes of Zirconium(IV) and Hafnium(IV) with Heteroscorpionate Ligands and the Hydrolysis of Such Complexes To Give a Zirconium Cluster#
A. Otero; J. Fernández-Baeza; A. Antiñolo; J. Tejeda; A. Lara-Sánchez; L. Sánchez-Barba; M. Fernández-López; I. López-Solera; Inorganic Chemistry 43 (2004) 1350–1358; doi:10.1021/ic035067c

data_4310606
_publ_contact_author
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Isabel L\'opez-Solera
Departamento de Qu\'imica In\'organica, Org\'anica y Bioqu\'imica
Facultad de Qu\'imicas
Universidad Castilla La Mancha
13071-Ciudad Real 
Spain
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_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#
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_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       '\w/2\q 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/[\s^2^(Fo^2^)+(0.0966P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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