Complexes of the [K(18-Crown-6)]+ Fragment with Bis(tetrazolyl)borate Ligands: Unexpected Boron-Nitrogen Bond Isomerism and Associated Enforcement of κ3-N,N',H-Ligand Chelation
Dongmei Lu; Charles H. Winter; Inorganic Chemistry 49 (2010) 5795–5797; doi:10.1021/ic100959j

data_4315990
_publ_contact_author             'Charles H. Winter'
_publ_contact_author_address
; Department of Chemistry
Wayne State University
5101 Cass Ave.
Detroit, Michigan 48202
U.S.A.
;
_publ_contact_author_email       chw@chem.wayne.edu
_publ_contact_author_phone       '313 577 5224'
_publ_section_title
;
 Complexes of the [K(18-Crown-6)]+ Fragment with Bis(tetrazolyl)borate
 Ligands: Unexpected Boron-Nitrogen Bond Isomerism and Associated
 Enforcement of \k3-N,N',H-Ligand Chelation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5795
_journal_page_last               5797
_journal_paper_doi               10.1021/ic100959j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C19.5 H36 B K N8 O6'
_chemical_formula_weight         528.47
_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-97
_cell_angle_alpha                101.349(2)
_cell_angle_beta                 94.052(2)
_cell_angle_gamma                105.252(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8464(3)
_cell_length_b                   10.0021(4)
_cell_length_c                   16.1443(6)
_cell_measurement_reflns_used    8116
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.3
_cell_volume                     1339.86(9)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_method       'Bruker APEX2'
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            36804
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.9296
_exptl_absorpt_correction_T_min  0.9163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomboids
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6583
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.4194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                6024
_reflns_number_total             6583
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100959j_si_001_3.cif
_cod_data_source_block           unod(5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 
;
_cod_original_formula_sum        'C19.50 H36 B K N8 O6'
_cod_database_code               4315990