(Borohydrido)(18-crown-6)potassium and (borohydrido)(dibenzo-18-crown-6)(tetrahydrofuran)potassium
Villiers, Claude; Thuéry, Pierre; Ephritikhine, Michel; Acta Crystallographica Section C 62 (2006) m275–m277; doi:10.1107/S0108270106016507

data_2015438
_publ_section_title
;
 (Borohydrido)(18-crown-6)potassium and
 (borohydrido)(dibenzo-18-crown-6)(tetrahydrofuran)potassium
;
_journal_coeditor_code           GZ3011
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m275
_journal_page_last               m277
_journal_paper_doi               10.1107/S0108270106016507
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[K (B H4) (C4 H8 O) (C20 H24 O6)]'
_chemical_formula_moiety         'C24 H36 B K O7'
_chemical_formula_sum            'C24 H36 B K O7'
_chemical_formula_weight         486.44
_chemical_name_systematic
;
(borohydrido)(1,4,7,10,13,16-hexaoxa-2,3:11,12-dibenzocyclooctadeca-
2,11-diene-\k^6^<i>O</i>)(tetrahydrofuran)potassium
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5611(4)
_cell_length_b                   9.9657(5)
_cell_length_c                   26.2779(15)
_cell_measurement_reflns_used    42072
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.95
_cell_volume                     2503.8(2)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  'SHELXTL and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'two \f and two \w scans with 2\% steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42072
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.246
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   0.08(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0789P)^2^+0.4778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                3880
_reflns_number_total             4737
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3011.cif
_cod_data_source_block           II
_cod_database_code               2015438
_cod_database_fobs_code          2015438