Derivatives of the Dimethylbis(2-pyridyl)borate(1-) Ion: Synthesis and Structure
Thomas G. Hodgkins; Douglas R. Powell; Inorganic Chemistry 35 (1996) 2140–2148; doi:10.1021/ic950775m

data_4324044
_publ_contact_author
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   Douglas R. Powell
   Department of Chemistry
   University of Wisconsin
   1101 University Ave. 
   Madison, WI  53706-1322  U.S.A.
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_publ_contact_author_email       powell@chem.wisc.edu
_publ_contact_author_fax         '608 262 0381'
_publ_contact_author_phone       '608 263 4694'
_publ_section_title
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 Derivatives of the Dimethylbis(2-pyridyl)borate(1-) Ion: Synthesis and
 Structure
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2140
_journal_page_last               2148
_journal_paper_doi               10.1021/ic950775m
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C24 H24 B2 N2'
_chemical_formula_weight         362.07
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.653(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0334(12)
_cell_length_b                   10.9169(9)
_cell_length_c                   22.981(2)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      10.4
_cell_volume                     2008.8(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            2930
_diffrn_reflns_theta_max         57.00
_diffrn_reflns_theta_min         3.86
_diffrn_standards_decay_%        0.0549
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0048(5)
_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   1.071
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_obs          0.0460
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.7903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1302
_refine_ls_wR_factor_obs         0.1221
_reflns_number_observed          2282
_reflns_number_total             2704
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic950775m_3.cif
_cod_data_source_block           compound_VI
_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^)+(0.0694P)^2^+0.7903P] 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^)+(0.0694P)^2^+0.7903P] 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               4324044