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_4317136
_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            'C45 H99 O9 Zr2'
_chemical_formula_weight         966.68
_chemical_name_common            'ZrOnep Hex'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 105.945(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7608(15)
_cell_length_b                   18.481(3)
_cell_length_c                   14.522(2)
_cell_measurement_reflns_used    2209
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      22.6657
_cell_measurement_theta_min      2.3747
_cell_volume                     2776.9(7)
_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_detector_area_resol_mean 8.3660
_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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17052
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'fine-focus tube'
_diffrn_source_type              'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.419
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_correction_T_min  0.356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             1042
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.166
_refine_diff_density_min         -0.601
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.739
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         7943
_refine_ls_number_restraints     803
_refine_ls_restrained_S_all      1.822
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.1097
_refine_ls_shift/su_max          5.463
_refine_ls_shift/su_mean         0.445
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3415
_refine_ls_wR_factor_ref         0.3793
_reflns_number_gt                6702
_reflns_number_total             7943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101205d_si_003_4.cif
_cod_data_source_block           9nv042s
_cod_database_code               4317136