Chiral C2 and C1 symmetric (cyclooctane-1,5-diyl)bis(2-pyrazolyl)borate complexes of potassium and thallium. Preparation, structures and solution behavior
Chisholm, Malcolm H.; Iyer, Suri S.; Streib, William E.; New Journal of Chemistry 24 (2000) 393–398; doi:10.1039/a906582b

data_5000333
_publ_section_title
;
 Chiral C2 and C1 symmetric (cyclooctane-1,5-diyl)bis(2-pyrazolyl)borate
 complexes of potassium and thallium. Preparation, structures and solution
 behavior
;
_journal_coden_ASTM              NJCHE5
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              393
_journal_page_last               398
_journal_paper_doi               10.1039/a906582b
_journal_volume                  24
_journal_year                    2000
_chemical_formula_moiety         'C30 H44 B1 N4 Tl1'
_chemical_formula_sum            'C30 H44 B N4 Tl'
_chemical_formula_weight         675.901
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 119.107(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.662(2)
_cell_length_b                   33.992(5)
_cell_length_c                   13.985(2)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    109
_cell_measurement_theta_max      14.3
_cell_measurement_theta_min      9.77
_cell_volume                     5674.1(16)
_diffrn_ambient_temperature      109
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'refurbished Picker diffractometer'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.072
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21679
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         25.0686
_diffrn_reflns_theta_min         3.0416
_diffrn_standards_decay_%        10.8
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    5.7093
_exptl_absorpt_correction_T_max  0.213
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'psi scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .10
_refine_diff_density_max         3.78
_refine_diff_density_min         -6.37
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   -0.02(1)
_refine_ls_extinction_coef       -0.000000004(4)
_refine_ls_extinction_expression
;
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   1.7485
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         16019
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.1594
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.07F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                16018
_reflns_number_total             20077
_reflns_threshold_expression     F>3.0\s(F)
_cod_duplicate_entry             7051234
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C30 H44 B1 N4 Tl1'
_cod_database_code               5000333