Isolation and Structural Characterization of Tetra-n-propyl Zirconate in Hydrocarbon Solution and the Solid State
Victor W. Day; Walter G. Klemperer; Margaret Mary Pafford; Inorganic Chemistry 40 (2001) 5738–5746; doi:10.1021/ic010776g

data_4320550
_publ_contact_author
;
       Walter Klemperer
       University of Illinois at Urbana
       Department of Chemistry
       MC-712
       Urbana, IL 61801
       U.S.A.
;
_publ_contact_author_email       wklemper@uiuc.edu
_publ_contact_author_fax         '217 333 2685'
_publ_contact_author_phone       '217 333 2995'
_publ_section_title
;
 Isolation and Structural Characterization of Tetra-n-propyl Zirconate in
 Hydrocarbon Solution and the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5738
_journal_page_last               5746
_journal_paper_doi               10.1021/ic010776g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C6 H14 O2 Zr0.5'
_chemical_formula_weight         163.78
_chemical_name_systematic
;
  ?
;
_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
_cell_angle_alpha                64.369(2)
_cell_angle_beta                 81.369(3)
_cell_angle_gamma                67.737(3)
_cell_formula_units_Z            8
_cell_length_a                   12.1153(12)
_cell_length_b                   12.6748(12)
_cell_length_c                   13.8687(12)
_cell_measurement_reflns_used    2078
_cell_measurement_temperature    293(2)
_cell_volume                     1776.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker SMART CCD Area Detector'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5833
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.8458
_exptl_absorpt_correction_T_min  0.6622
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'rectangular parallelepiped'
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_description       colorless
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.099
_refine_ls_goodness_of_fit_obs   1.231
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.297
_refine_ls_restrained_S_obs      1.227
_refine_ls_R_factor_all          0.1600
_refine_ls_R_factor_obs          0.0968
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.1123P)^2^+4.6061P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3392
_refine_ls_wR_factor_obs         0.2350
_reflns_number_observed          2228
_reflns_number_total             4049
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010776g.cif
_cod_data_source_block           wks2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.1123P)^2^+4.6061P] where P=3D(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=3D1/[\s^2^(Fo^2^)+(0.1123P)^2^+4.6061P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C6 H14 O2 Zr0.50'
_cod_database_code               4320550