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_4320912
_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            'C41 H69 Cl18 Mn N12 Zr6'
_chemical_formula_weight         1956.16
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.73(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.664(4)
_cell_length_b                   17.468(4)
_cell_length_c                   23.591(5)
_cell_measurement_temperature    293(2)
_cell_volume                     7438(3)
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            45754
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    1.664
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_F_000             4124
_refine_diff_density_max         1.470
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.920
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         15562
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.920
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_obs          0.0360
_refine_ls_shift/esd_max         13.372
_refine_ls_shift/esd_mean        0.085
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0988
_refine_ls_wR_factor_obs         0.0886
_reflns_number_observed          9494
_reflns_number_total             15562
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9913785_2.cif
_cod_data_source_block           Im5Zr6MnCl18.C7H8.2CH3CN
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.0466P)^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^)+(0.0466P)^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        7438.1(26)
_cod_database_code               4320912