Synthesis, Structure, and Reactivity of [Zr6Cl18H5]2-, the First Paramagnetic Species of Its Class
Linfeng Chen; F. Albert Cotton; Inorganic Chemistry 35 (1996) 7364–7369; doi:10.1021/ic960454q

data_4323984
_publ_section_title
;
 Synthesis, Structure, and Reactivity of [Zr6Cl18H5]2-, the First
 Paramagnetic Species of Its Class
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7364
_journal_page_last               7369
_journal_paper_doi               10.1021/ic960454q
_journal_volume                  35
_journal_year                    1996
_chemical_compound_source
;
reaction of [Ph4P]4[Zr6Cl18H5] with TiCl4
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         '2(C24 H20 P 1+),H6 Cl18 Zr6 2-'
_chemical_formula_structural     '[(C6 H5)4 P]3 [Zr6 Cl18 H6]'
_chemical_formula_sum            'C48 H46 Cl18 P2 Zr6'
_chemical_formula_weight         1870.21
_chemical_name_systematic
; 
 bis(tetraphenylphosphonium) dodecakis-/m-chloro-hexachloro-
 hexahydrido-hexa-zirconium 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   28.546(3)
_cell_length_b                   28.546(3)
_cell_length_c                   27.679(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     19533(3)
_computing_cell_refinement       'Enraf-Nonius CAD4 version 5.0'
_computing_data_collection       'Enraf-Nonius CAD4 version 5.0'
_computing_data_reduction        'Enraf-Nonius CAD4 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       'omega - theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo Ka'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.1399
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            4699
_diffrn_reflns_theta_max         19.93
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        6.6
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  1.0903
_exptl_absorpt_correction_T_min  0.9344
_exptl_absorpt_correction_type   'empirical via psi scans'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rhomboidal
_exptl_crystal_F_000             10920
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.032
_refine_ls_goodness_of_fit_obs   1.178
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         4028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_restrained_S_obs      1.178
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_obs          0.0496
_refine_ls_shift/esd_max         -0.012
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1211
_refine_ls_wR_factor_obs         0.0938
_reflns_number_observed          2104
_reflns_number_total             4028
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960454q_2.cif
_cod_data_source_block           '[Ph4P]2[Zr6Cl18H5](2a)'
_cod_depositor_comments
;
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^)+(0.0400P)^2^+0.0000P] 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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4323984