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_4323548
_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 followed by addition of [Ph4P]Cl
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         '4(C24 H20 P),Zr6 Cl18 H5, 4(C7 H8)'
_chemical_formula_structural     '[(C6 H5)4 P]3 [Zr6 Cl18 H5] 4(C6 H5 C H3)'
_chemical_formula_sum            'C100 H97 Cl18 P3 Zr6'
_chemical_formula_weight         2577.11
_chemical_melting_point          ?
_chemical_name_systematic
; 
 tris(tetraphenylphosphonium) dodecakis-\m-chloro-hexachloro-
 pentahydrido-hexa-zirconium  tetrakis(toluene solvate)
;
_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   'difmap for cluster hydrogen,geom for other'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.39(3)
_cell_angle_beta                 94.19(3)
_cell_angle_gamma                82.59(1)
_cell_formula_units_Z            2
_cell_length_a                   14.501(5)
_cell_length_b                   26.630(9)
_cell_length_c                   14.049(5)
_cell_measurement_reflns_used    244
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.0
_cell_volume                     5365(3)
_computing_cell_refinement       Madnes
_computing_data_collection       'MicroVax 3900'
_computing_data_reduction        absurd
_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 FAST'
_diffrn_measurement_method       'frame data from omega scans'
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28263
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1174
_refine_ls_number_reflns         16500
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_obs          0.0694
_refine_ls_shift/esd_max         0.018
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+74.0691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1683
_refine_ls_wR_factor_obs         0.1424
_reflns_number_observed          11345
_reflns_number_total             16507
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960173i_3.cif
_cod_data_source_block           2a.4C6H5CH3
_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.

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^)+(0.0208P)^2^+74.0691P] 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^)+(0.0208P)^2^+74.0691P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323548