Synthesis and Structural Characterization of Compounds Containing the [Zr6Cl18H5]3- Cluster Anion. Determination of the Number of Cluster Hydrogen Atoms
Linfeng Chen; F. Albert Cotton; William A. Wojtczak; Inorganic Chemistry 36 (1997) 4047–4054; doi:10.1021/ic960173i

data_4323550
_publ_section_title
;
 Synthesis and Structural Characterization of Compounds Containing the
 [Zr6Cl18H5]3- Cluster Anion. Determination of the Number of Cluster
 Hydrogen Atoms
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4047
_journal_page_last               4054
_journal_paper_doi               10.1021/ic960173i
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source
;
reduction of ZrCl4 with HSnBu3 followd by addition of [Pr4N]Cl 
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         '3(C12 H28 N), Zr6 Cl18 H5'
_chemical_formula_structural     '[(C3 H7)4 N]3 [Zr6 Cl18 H5]'
_chemical_formula_sum            'C36 H89 Cl18 N3 Zr6'
_chemical_formula_weight         1749.52
_chemical_melting_point          ?
_chemical_name_systematic
; 
 tris(tetrapropylammonium)-dodecakis(\m-chloro)-hexachloro-
 pentahydrido-hexa-zirconium 
;
_space_group_IT_number           229
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_atom_sites_solution_hydrogens   'difmap for cluster hydrogen'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.093(3)
_cell_length_b                   15.093(3)
_cell_length_c                   15.093(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      16
_cell_volume                     3438.2(12)
_computing_cell_refinement       'Enraf-Nonius CAD4 Version 5.0'
_computing_data_collection       'Enraf-Nonius CAD4 Version 5.0'
_computing_data_reduction        'Enraf-Nonius SDP'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            531
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        1.1
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.227
_refine_ls_hydrogen_treatment    'refall for cluster hydrogen'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_restrained_S_obs      1.227
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+14.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1186
_refine_ls_wR_factor_obs         0.1092
_reflns_number_observed          329
_reflns_number_total             531
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960173i_5.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_geom_bond_publ_flag' value
'Y' changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (4 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z 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=1/[\s^2^(Fo^2^)+(0.0385P)^2^+14.0000P] where P=(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=1/[\s^2^(Fo^2^)+(0.0385P)^2^+14.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3438(1)
_cod_database_code               4323550