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_4331847
_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            'C40 H80 O10 Zr2'
_chemical_formula_weight         903.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.21(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.191(16)
_cell_length_b                   9.753(8)
_cell_length_c                   26.796(19)
_cell_measurement_reflns_used    781(I>10sigma(I))
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18.00
_cell_measurement_theta_min      1.60
_cell_volume                     4952(7)
_computing_cell_refinement       'Bruker SAINTPLUS'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL-NT'
_computing_publication_material  'Bruker SHELXTL-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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0803
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11463
_diffrn_reflns_theta_full        18.00
_diffrn_reflns_theta_max         18.00
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.9333
_exptl_absorpt_correction_T_min  0.8002
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3408
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_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0842
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1693P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2316
_refine_ls_wR_factor_ref         0.2605
_reflns_number_gt                1942
_reflns_number_total             3408
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051674jsup2.cif
_cod_data_source_block           zrppthd1
_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_cell_volume        4952(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4331847