Studies on Mixed β-Diketonate/Isopropoxide Compounds of Zirconium and Hafnium, the X-ray Single-Crystal Structures of [M2(OPri)6(tmhd)2] (M = Zr, Hf): Some Chemistry Important in the MOCVD of Oxides
Kirsty A. Fleeting; Paul O'Brien; David J. Otway; Andrew J. P. White; David J. Williams; Anthony C. Jones; Inorganic Chemistry 38 (1999) 1432–1437; doi:10.1021/ic980690w

data_4321859
_publ_section_title
;
 Studies on Mixed \b-Diketonate/Isopropoxide Compounds of Zirconium and
 Hafnium, the X-ray Single-Crystal Structures of [M2(OPri)6(tmhd)2] (M =
 Zr, Hf): Some Chemistry Important in the MOCVD of Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1432
_journal_page_last               1437
_journal_paper_doi               10.1021/ic980690w
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C40 H80 O10 Zr2'
_chemical_formula_weight         903.48
_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                69.731(12)
_cell_angle_beta                 74.412(14)
_cell_angle_gamma                71.470(12)
_cell_formula_units_Z            1
_cell_length_a                   10.629(2)
_cell_length_b                   11.204(2)
_cell_length_c                   11.858(2)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.99
_cell_volume                     1235.9(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_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      203(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5907
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        11.61
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.8280
_exptl_absorpt_correction_T_min  0.7592
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       blocks
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.67
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5598
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.095
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_obs          0.0411
_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/[\s^2^(Fo^2^)+(0.0498P)^2^+0.5126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1065
_refine_ls_wR_factor_obs         0.0975
_reflns_number_observed          4771
_reflns_number_total             5603
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980690w_1.cif
_cod_data_source_block           POB9709
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.5126P] 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^)+(0.0498P)^2^+0.5126P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321859