Homoleptic zirconium amidates: single source precursors for the aerosol-assisted chemical vapour deposition of ZrO2
Amanda L. Catherall; Michael S. Hill; Andrew L. Johnson; Gabriele Kociok-Kohn; Mary F. Mahon; Journal of Materials Chemistry C 4 (2016) 10731–10739; doi:10.1039/C6TC03631G

data_7235120
_publ_section_title
;
 Homoleptic zirconium amidates: single source precursors for the
 aerosol-assisted chemical vapour deposition of ZrO2
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              10731
_journal_page_last               10739
_journal_paper_doi               10.1039/C6TC03631G
_journal_volume                  4
_journal_year                    2016
_chemical_formula_moiety         'C29 H60 N4 O3 Zr'
_chemical_formula_sum            'C29 H60 N4 O3 Zr'
_chemical_formula_weight         604.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 90.090(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8077(5)
_cell_length_b                   17.3778(8)
_cell_length_c                   18.1390(9)
_cell_measurement_reflns_used    7499
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.8560
_cell_measurement_theta_min      3.5600
_cell_volume                     3406.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -18.00   9.00   1.00   75.00    --  -14.16 -99.00  90.00   27
  2  \w    -41.00  51.00   1.00   75.00    --  -14.16  77.00  60.00   92
  3  \w    -82.00  13.00   1.00   75.00    --  -14.16 -77.00 -60.00   95
  4  \w     -7.00  22.00   1.00   75.00    --  -14.16 -99.00-180.00   29
  5  \w    -27.00  49.00   1.00   75.00    --  -14.16  38.00-150.00   76
  6  \w     -1.00  24.00   1.00   75.00    --   14.79  57.00-150.00   25
  7  \w     34.00  59.00   1.00   75.00    --   14.79-178.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25934
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.068
_diffrn_reflns_theta_min         3.369
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.132
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6663
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+2.2605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5467
_reflns_number_total             6663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            J-Mater-Chem-C-2016-4-10731.cif
_cod_data_source_block           e16msh4
_cod_original_cell_volume        3406.7(3)
_cod_database_code               7235120