Molecular Aggregates of Nitrate Ion with the Tetravalent Lewis Acid Host 12-Mercuracarborand-4: Novel Trihapto Coordination of NO3-
Alfred A. Zinn; Carolyn B. Knobler; David E. Harwell; M. Frederick Hawthorne; Inorganic Chemistry 38 (1999) 2227–2230; doi:10.1021/ic9811244

data_4321955
_publ_contact_author
;
Hawthorne, M. F.,
Department of Chemistry and Biochemistry,
University of California,
Los Angeles, CA 90095-1569.  USA
;
_publ_contact_author_email       KNOBLERH@CHEM.UCLA.EDU
_publ_contact_author_fax         310-825-5490
_publ_contact_author_phone       310-825-7378
_publ_section_title
;
 Molecular Aggregates of Nitrate Ion with the Tetravalent Lewis Acid Host
 12-Mercuracarborand-4: Novel Trihapto Coordination of NO3-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2227
_journal_page_last               2230
_journal_paper_doi               10.1021/ic9811244
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C32 H88 B40 Hg4 K2 N2 O18'
_chemical_formula_weight         2102.00
_chemical_name_systematic
; 
[12]mercuracarborand-4.3KNO~3~.K-18-crown-6
;
_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                102.55(2)
_cell_angle_beta                 100.63(3)
_cell_angle_gamma                109.075(10)
_cell_formula_units_Z            1
_cell_length_a                   12.4270(7)
_cell_length_b                   12.8492(7)
_cell_length_c                   13.6340(8)
_cell_measurement_reflns_used    66
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.25
_cell_measurement_theta_min      4.85
_cell_volume                     1929.8(5)
_computing_cell_refinement       'UCLA package'
_computing_data_collection       'UCLA package'
_computing_data_reduction        'UCLA package'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    Patterson
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Crystal Logic'
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1155
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10994
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        18%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.095
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_description       plate
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.420
_refine_diff_density_min         -1.636
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.960
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         8450
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.998
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.1751
_refine_ls_R_factor_obs          0.0672
_refine_ls_shift/esd_max         0.031
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+8.4238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2377
_refine_ls_wR_factor_obs         0.1672
_reflns_number_observed          4660
_reflns_number_total             10994
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9811244_2.cif
_cod_data_source_block           COMPLEX2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+8.4238P] 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^)+(0.1011P)^2^+8.4238P] 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        1929.8(2)
_cod_database_code               4321955