Chemistry of 2,2,6,6,-Tetramethyl-3,5-heptanedione (Hthd) Modification of Zirconium and Hafnium Propoxide Precursors
Spijksma, Gerald I.; Bouwmeester, Henny J. M.; Blank, Dave H. A.; Fischer, Andreas; Henry, Marc; Kessler, Vadim G.; Inorganic Chemistry 45 (2006) 4938–4950; doi:10.1021/ic051674j

data_4331851
_publ_section_title
;
 Chemistry of 2,2,6,6,-Tetramethyl-3,5-heptanedione (Hthd) Modification of
 Zirconium and Hafnium Propoxide Precursors
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4938
_journal_page_last               4950
_journal_paper_doi               10.1021/ic051674j
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C44 H76 O8 Zr'
_chemical_formula_weight         824.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.550(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.545(6)
_cell_length_b                   11.275(3)
_cell_length_c                   19.763(5)
_cell_measurement_reflns_used    494(I>10sigma(I))
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18.00
_cell_measurement_theta_min      1.81
_cell_volume                     4816(2)
_computing_cell_refinement       'Bruker SAINTPLUS'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXYL-NT'
_computing_publication_material  'Bruker SHELXYL-NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART CCD 1k'
_diffrn_measurement_method       'Bruker SMART'
_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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10785
_diffrn_reflns_theta_full        18.00
_diffrn_reflns_theta_max         18.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8645
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         3275
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+21.4816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2261
_reflns_number_gt                2282
_reflns_number_total             3275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051674jsup7.cif
_cod_data_source_block           zrthd4m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               4331851