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_4323983
_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 py'
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'C24 H20 P,Zr Cl5 N C5 H5'
_chemical_formula_structural     (Ph4P)[ZrCl5(py)]
_chemical_formula_sum            'C29 H25 Cl5 N P Zr'
_chemical_formula_weight         686.94
_chemical_name_systematic
; 
 (tetraphenylphosphnium)[pentachloro-pyridine-zirconium] 
;
_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                90.000(7)
_cell_angle_beta                 91.542(6)
_cell_angle_gamma                90.000(7)
_cell_formula_units_Z            4
_cell_length_a                   10.3990(7)
_cell_length_b                   16.491(2)
_cell_length_c                   17.654(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      45
_cell_volume                     3026.4(5)
_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       'rigaku afc5r'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4775
_diffrn_reflns_theta_max         60.02
_diffrn_reflns_theta_min         3.67
_diffrn_standards_decay_%        22.4
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.689
_exptl_absorpt_correction_T_max  0.4141
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.264
_refine_diff_density_min         -2.098
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.028
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_obs          0.0672
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+57.2929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1767
_refine_ls_wR_factor_obs         0.1551
_reflns_number_observed          3550
_reflns_number_total             4498
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960454q_1.cif
_cod_data_source_block           '[Ph4P][Zr5(py)](6a)'
_cod_depositor_comments
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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^)+(0.0214P)^2^+57.2929P] 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^)+(0.0214P)^2^+57.2929P] 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               4323983