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_4116871
_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            'C40 H30 B Cl14 N8 Zr6'
_chemical_formula_weight         1677.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.8920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5999(3)
_cell_length_b                   21.2298(5)
_cell_length_c                   19.8292(5)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    213(2)
_cell_volume                     6014.2(2)
_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 (Bruker)'
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13947
_diffrn_reflns_theta_max         27.76
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_description       plate
_exptl_crystal_F_000             3236
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.144
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         6083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_obs          0.0455
_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^)+(0.0149P)^2^+53.1476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1036
_refine_ls_wR_factor_obs         0.0863
_reflns_number_observed          4487
_reflns_number_total             6086
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja981736n_2.cif
_cod_data_source_block           '[pyH][(Zr6BCl12)Cl2(py)4]3py'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+53.1476P] 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^)+(0.0149P)^2^+53.1476P] 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               4116871