Structurally characterized carboxylic acid modified zirconium alkoxides for the production of zirconium oxide thin films
Timothy J. Boyle; Leigh Anna M. Ottley; Mark A. Rodriguez; Polyhedron 24 (2005) 1727–1738; doi:10.1016/j.poly.2005.05.005

data_1512908
_publ_section_title
;
 Structurally characterized carboxylic acid modified zirconium alkoxides
 for the production of zirconium oxide thin films
;
_journal_issue                   13
_journal_name_full               Polyhedron
_journal_page_first              1727
_journal_page_last               1738
_journal_paper_doi               10.1016/j.poly.2005.05.005
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C32 H74 O11 Zr2'
_chemical_formula_weight         817.35
_chemical_name_common            '(5) Zr2(OBc)(OPri)7(HOPri)*(HOPri)'
_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                76.786(4)
_cell_angle_beta                 86.427(4)
_cell_angle_gamma                61.086(3)
_cell_formula_units_Z            2
_cell_length_a                   12.737(3)
_cell_length_b                   12.943(3)
_cell_length_c                   15.756(4)
_cell_measurement_temperature    168(2)
_cell_volume                     2209.9(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0170
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13745
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6360
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+8.6237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                5529
_reflns_number_total             6360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2005-1727.cif
_cod_data_source_block           lo01s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

  The following markup was performed in this entry:

  a) disordered atoms were assigned to two different disorder
  assempblies and distributed into two disorder groups;

  b) _atom_site_attached_hydrogens were added to atoms missing
  explicit hydrogens, in the places where the presence of a hydrogen
  was evident from the chemistry.

  After these updates, the computed, declared and published chmical
  formulae all are the same.

  Saulius Gra\<zulis
  2013-12-06
;
_cod_original_cell_volume        2210.0(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512908