Series of Comparable Dinuclear Group 4 Neo-pentoxide Precursors for Production of pH Dependent Group 4 Nanoceramic Morphologies
Timothy J. Boyle; Leigh Anna M. Ottley; Sarah M. Hoppe; Charles F. Campana; Inorganic Chemistry 49 (2010) 10798–10808; doi:10.1021/ic101205d

data_4317137
_publ_contact_author_address
;
Sandia National Laboratories
Advanced Materials Laboratory'
1001 University Boulevard NE'
Albuquerque, NM 87106
;
_publ_contact_author_email
;
tjboyle@sandia.gov
;
_publ_contact_author_fax
;
(505) 272-7336
;
_publ_contact_author_name        'Timothy M. Boyle'
_publ_contact_author_phone
;
(505) 272-7625
;
_publ_section_title
;
 Series of Comparable Dinuclear Group 4 Neo-pentoxide Precursors for
 Production of pH Dependent Group 4 Nanoceramic Morphologies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10798
_journal_page_last               10808
_journal_paper_doi               10.1021/ic101205d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C98 H216 Hf6 O22'
_chemical_formula_weight         2817.65
_chemical_name_common            'HfONep H2O'
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   18.867(3)
_cell_length_b                   18.867(3)
_cell_length_c                   23.072(9)
_cell_measurement_temperature    173.(2)
_cell_volume                     7112(3)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'APEX2 v2010.9 (Bruker, 2010)'
_computing_publication_material  'APEX2 v2010.9 (Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48934
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.25
_diffrn_source                   'fine-focus tube'
_diffrn_source_type              'fine-focus tube'
_exptl_absorpt_coefficient_mu    4.409
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2824
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
;
_refine_diff_density_max         1.490
_refine_diff_density_min         -0.681
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4320
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+22.2977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                4049
_reflns_number_total             4320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101205d_si_003_5.cif
_cod_data_source_block           10ap131s
_cod_original_cell_volume        7112.(3)
_cod_database_code               4317137