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_4323546
_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
;
addition of [Ph4P]I to the brown solid from reaction of ZrCl4 with HSnBu3' 
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
3(C24 H20 P 1+),Zr6 Cl17.19 I0.81 H5 3-,3(C H2 Cl2),C7 H8
;
_chemical_formula_structural
;
[(C6 H5)4 P]3 [Zr6 Cl17.19 I0.81 H5] 3(C H2 Cl2) (C6 H5 C H3)
;
_chemical_formula_sum            'C82 H79 Cl23.19 I0.81 P3 Zr6'
_chemical_formula_weight         2629.79
_chemical_melting_point          ?
_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   'difmap for cluster hydrogen,geom for others'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.22(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.786(5)
_cell_length_b                   19.071(4)
_cell_length_c                   27.397(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      11.5
_cell_volume                     10338(4)
_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      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w--\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.1129
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14817
_diffrn_reflns_theta_max         22.95
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        30.5
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.8215
_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_description       cubic
_exptl_crystal_F_000             5173
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.48
_refine_diff_density_max         1.033
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         14333
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.078
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_obs          0.0582
_refine_ls_shift/esd_max         0.052
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+96.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1680
_refine_ls_wR_factor_obs         0.1226
_reflns_number_observed          7775
_reflns_number_total             14337
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960173i_1.cif
_cod_data_source_block           3.3CH2Cl2.C6H5CH3
_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^)+(0.0237P)^2^+96.1104P] 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^)+(0.0237P)^2^+96.1104P] 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        10337(4)
_cod_original_formula_sum        'C82 H5 H74 Cl23.19 I0.81 P3 Zr6'
_cod_database_code               4323546