Synthesis and structure of mixed isopropoxide–β-ketoester and β-ketoamide zirconium complexes: Potential precursors for MOCVD of ZrO~2~
Patil, Urmila; Winter, Manuela; Becker, Hans-Werner; Devi, Anjana; Journal of Materials Chemistry 13 (2003) 2177–2184; doi:10.1039/b304419j

data_7204674
_publ_section_title
;
 Synthesis and structure of mixed isopropoxide--\b-ketoester and \b-ketoamide
 zirconium complexes: Potential precursors for MOCVD of ZrO~2~
;
_journal_coden_ASTM              JMACEP
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2177
_journal_page_last               2184
_journal_paper_doi               10.1039/b304419j
_journal_volume                  13
_journal_year                    2003
_chemical_formula_sum            'C34 H68 O12 Zr2'
_chemical_formula_weight         851.32
_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                74.74(2)
_cell_angle_beta                 89.86(2)
_cell_angle_gamma                89.86(3)
_cell_formula_units_Z            2
_cell_length_a                   10.977(3)
_cell_length_b                   13.192(4)
_cell_length_c                   16.218(5)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2265.7(12)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Bruker axs SHELXL-PLUS'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker axs CCD 1000'
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.1961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12972
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7891
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1890
_refine_ls_wR_factor_ref         0.2415
_reflns_number_gt                5157
_reflns_number_total             7891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304419j.txt
_cod_data_source_block           3t
_cod_original_cell_volume        2265.7(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204674