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_4321860
_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 Hf2 O10'
_chemical_formula_weight         1078.02
_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                69.369(9)
_cell_angle_beta                 74.170(9)
_cell_angle_gamma                71.405(10)
_cell_formula_units_Z            1
_cell_length_a                   10.5798(11)
_cell_length_b                   11.1755(14)
_cell_length_c                   11.8443(13)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.30
_cell_volume                     1221.7(3)
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4196
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        13.12
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.292
_exptl_absorpt_correction_T_max  0.7279
_exptl_absorpt_correction_T_min  0.4721
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       'platy rhombs'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.157
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.050
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3968
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_obs          0.0402
_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^)+(0.0445P)^2^+0.6352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0984
_refine_ls_wR_factor_obs         0.0922
_reflns_number_observed          3387
_reflns_number_total             3968
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980690w_2.cif
_cod_data_source_block           POB9711
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.6352P] 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^)+(0.0445P)^2^+0.6352P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1221.7(2)
_cod_original_formula_sum        'C40 H80 O10 Hf2'
_cod_database_code               4321860