Chloroaluminate Ionic Liquids as Reagents for Isolating Soluble Hexanuclear Zirconium Halide Cluster Compounds
Dong Sun; Timothy Hughbanks; Inorganic Chemistry 39 (2000) 1964–1968; doi:10.1021/ic9913785

data_4320913
_publ_section_title
;
 Chloroaluminate Ionic Liquids as Reagents for Isolating Soluble
 Hexanuclear Zirconium Halide Cluster Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1964
_journal_page_last               1968
_journal_paper_doi               10.1021/ic9913785
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C24 H44 B Cl18 N8 Zr6'
_chemical_formula_weight         1640.90
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                98.003(9)
_cell_angle_beta                 98.800(9)
_cell_angle_gamma                112.877(9)
_cell_formula_units_Z            2
_cell_length_a                   11.785(2)
_cell_length_b                   11.8925(15)
_cell_length_c                   21.006(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2615.9(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4028
_diffrn_reflns_theta_max         17.50
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    2.102
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_F_000             1590
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.076
_refine_ls_goodness_of_fit_obs   1.147
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.089
_refine_ls_restrained_S_obs      1.164
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_obs          0.0357
_refine_ls_shift/esd_max         -0.361
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0899
_refine_ls_wR_factor_obs         0.0807
_reflns_number_observed          2473
_reflns_number_total             3289
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9913785_3.cif
_cod_data_source_block           Im4Zr6BCl18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0401P)^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^)+(0.0401P)^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_cell_volume        2616.0(6)
_cod_database_code               4320913