Probing the Coordination Chemistry of [Zr6BCl12]+: A Cluster Especially Amenable to NMR Study
Xiaobing Xie; Joseph H. Reibenspies; Timothy Hughbanks; Journal of the American Chemical Society 120 (1998) 11391–11400; doi:10.1021/ja981736n

data_4116870
_publ_section_title
;
 Probing the Coordination Chemistry of [Zr6BCl12]+: A Cluster Especially
 Amenable to NMR Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11391
_journal_page_last               11400
_journal_paper_doi               10.1021/ja981736n
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C31 H25 B Cl13 N8 Zr6'
_chemical_formula_weight         1528.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4268(2)
_cell_length_b                   25.82580(10)
_cell_length_c                   14.5918(2)
_cell_measurement_temperature    213(2)
_cell_volume                     5059.82(10)
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'SMART CCD (Brucker)'
_diffrn_measurement_method       omega
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22863
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.911
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2932
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.206
_refine_ls_goodness_of_fit_obs   1.244
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5686
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.282
_refine_ls_restrained_S_obs      1.346
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_obs          0.0625
_refine_ls_shift/esd_max         -2.037
_refine_ls_shift/esd_mean        0.067
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+43.5927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1228
_refine_ls_wR_factor_obs         0.1038
_reflns_number_observed          3922
_reflns_number_total             5692
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja981736n_1.cif
_cod_data_source_block           '[(Zr6BCl12)Cl(py)5]3CH3CN'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+43.5927P] 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^)+(0.0170P)^2^+43.5927P] 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               4116870