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_7052465
_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_sum            'C46 H80 B K N4 O4'
_chemical_formula_weight         803.075
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4597(19)
_cell_length_b                   21.273(2)
_cell_length_c                   10.8452(11)
_cell_measurement_reflns_used    176
_cell_measurement_temperature    107.
_cell_measurement_theta_max      12.27
_cell_measurement_theta_min      9.61
_cell_volume                     4489.5(8)
_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      107.15
_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  0.057
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8532
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         24.9894
_diffrn_reflns_theta_min         3.05734
_diffrn_standards_decay_%        1.4
_diffrn_standards_interval_count 400
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.1644
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'partially redisolved'
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          '.30 .30 .35'
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .30
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details
;
absolute structure based on refinement using both possibilites
;
_refine_ls_extinction_coef       0.00000060(7)
_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   1.4135
_refine_ls_hydrogen_treatment    'fixed, idealized'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         5894
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.0215
_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         0.0484
_reflns_number_gt                5181
_reflns_number_total             7876
_reflns_threshold_expression     F^2^>2.33\s(F^2^)
_cod_duplicate_entry             7051232
_cod_data_source_file            a906582b.txt
_cod_data_source_block           MSC98047
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_ambient_temperature' value '-166.' was changed to '107.15' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        4489.6(8)
_cod_original_formula_sum        'C46 H80 B1 K1 N4 O4'
_cod_database_code               7052465