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_5000332
_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         ?
_chemical_formula_sum            'C42 H68 B K N4 O3'
_chemical_formula_weight         726.936
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                93.05(2)
_cell_angle_beta                 115.304(19)
_cell_angle_gamma                69.30(2)
_cell_formula_units_Z            2
_cell_length_a                   12.445(5)
_cell_length_b                   17.492(7)
_cell_length_c                   11.194(4)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    103.
_cell_measurement_theta_max      12.07
_cell_measurement_theta_min      9.94
_cell_volume                     2046.9(15)
_diffrn_ambient_temperature      103.
_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  0.121
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12419
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         28.0497
_diffrn_reflns_theta_min         3.03548
_diffrn_standards_decay_%        .2
_diffrn_standards_interval_count 400
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.1718
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .30
_refine_diff_density_max         0.5
_refine_diff_density_min         -0.61
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       0.00000083(17)
_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   1.8758
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         3312
_refine_ls_R_factor_gt           0.072
_refine_ls_shift/su_max          0.0387
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.03F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                3556
_reflns_number_total             7199
_reflns_threshold_expression     F^2^>2.33\s(F^2^)
_cod_duplicate_entry             7051233
_cod_original_formula_sum        'C42 H68 B1 K1 N4 O3'
_cod_database_code               5000332