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_4321954
_publ_contact_author
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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
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 Molecular Aggregates of Nitrate Ion with the Tetravalent Lewis Acid Host
 12-Mercuracarborand-4: Novel Trihapto Coordination of NO3-
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_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            'C35 H98 B40 Hg4 K2 N2 O21'
_chemical_formula_weight         2196.11
_chemical_name_common
; 
[12]mercuracarborand-4 . 2 K-18-crown-6 . 2 NO~3~ . 2 H~2~O . 1 (CH~3~)~2~C=O
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'heavy atom methods'
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3600(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9919(9)
_cell_length_b                   16.4156(7)
_cell_length_c                   23.3225(10)
_cell_measurement_reflns_used    99
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.2
_cell_measurement_theta_min      4.8
_cell_volume                     8382.8(6)
_computing_cell_refinement       'UCLA package'
_computing_data_collection       'UCLA package'
_computing_data_reduction        'REDUCE (UCLA crystallographic package)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Huber (Crystal Logic)'
_diffrn_radiation_detector       scintillation
_diffrn_radiation_detector_dtime 3.5
_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  0.1463
_diffrn_reflns_av_sigmaI/netI    0.1282
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14772
_diffrn_reflns_reduction_process 'modified Lehmann-Larsen algorithm'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.460
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4192
_exptl_crystal_preparation       capillary
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         2.335
_refine_diff_density_min         -2.432
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       0.00002(2)
_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   1.120
_refine_ls_goodness_of_fit_obs   1.361
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         10568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_restrained_S_obs      1.361
_refine_ls_R_factor_all          0.2134
_refine_ls_R_factor_obs          0.0712
_refine_ls_shift/esd_max         -1.491
_refine_ls_shift/esd_mean        0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+17.7800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2837
_refine_ls_wR_factor_obs         0.1920
_reflns_number_observed          5460
_reflns_number_total             14770
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9811244_1.cif
_cod_data_source_block           compound
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+17.7800P] 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^)+(0.0940P)^2^+17.7800P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321954