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_4323987
_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]3[Zr6Cl18H5] with H+, crystallized from MeCN-Et2O
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         '(C24 H20 P)2,Zr Cl6,4(C2 H3 N)'
_chemical_formula_structural     '[(C6 H5)4 P 1+]2 [Zr Cl6 2-] 4(C H3 C N)'
_chemical_formula_sum            'C56 H52 Cl6 N4 P2 Zr'
_chemical_formula_weight         1146.88
_chemical_name_systematic
; 
 bis(tetraphenylphosphnium) hexachloro-zirconium(IV) 
 tetrakis(acetonitrile solvate) 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.50(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.595(1)
_cell_length_b                   19.566(3)
_cell_length_c                   15.049(1)
_cell_measurement_reflns_used    247
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.0
_cell_volume                     2794.2(6)
_computing_cell_refinement       Madnes
_computing_data_collection       'MicroVAx 3900'
_computing_data_reduction        absurd
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16222
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.110
_refine_ls_goodness_of_fit_obs   1.124
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_restrained_S_obs      1.124
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_obs          0.0815
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+15.7413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1482
_refine_ls_wR_factor_obs         0.1454
_reflns_number_observed          4535
_reflns_number_total             4818
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960454q_5.cif
_cod_data_source_block           '[Ph4P]2[ZrCl6].4MeCN(5a.4MeCN)'
_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^)+(0.0113P)^2^+15.7413P] 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^)+(0.0113P)^2^+15.7413P] 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               4323987