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_7051231
_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 B K N4, 2(C4 H8 O), C4 H10 O'
_chemical_formula_sum            'C42 H70 B K N4 O3'
_chemical_formula_weight         728.952
_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'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.1 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 110.465(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.064(3)
_cell_length_b                   18.385(6)
_cell_length_c                   11.155(3)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    105
_cell_measurement_theta_max      16.97
_cell_measurement_theta_min      10.73
_cell_volume                     2125.8(11)
_computing_cell_refinement       'XTEL, local package'
_computing_data_collection       'NPS, local program'
_computing_data_reduction        'XTEL, local package'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    MULTAN78
_diffrn_ambient_temperature      105
_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  0.041
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9550
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         25.1025
_diffrn_reflns_theta_min         3.1453
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.1657
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular tetrahedron'
_exptl_crystal_F_000             796
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .30
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.99
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   -0.02(10)
_refine_ls_extinction_coef       -0.0000002(2)
_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   1.6176
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5464
_refine_ls_R_factor_gt           0.094
_refine_ls_shift/su_max          0.1473
_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         0.0904
_reflns_number_gt                5463
_reflns_number_total             7514
_reflns_threshold_expression     F>3.0\s(F)
_cod_data_source_file            a906582b.txt
_cod_data_source_block           MSC98048
_cod_original_cell_volume        2125.8(12)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7051231