Crystal structure of (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane-κ 8 N 2, O 6) potassium cyclopentadienide, [K([2.2.2]crypt)]Cp, C23H41KN2O6
Fischer, Christina; Klein, Wilhelm; Fässler, Thomas F.; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1259–1261; doi:10.1515/ncrs-2021-0296

data_8104580
_publ_section_title
;
 Crystal structure of
 (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane-\k 8 N 2, O
 6) potassium cyclopentadienide, [K([2.2.2]crypt)]Cp, C23H41KN2O6
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1259
_journal_page_last               1261
_journal_paper_doi               10.1515/ncrs-2021-0296
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C18 H36 K N2 O6, C5 H5'
_chemical_formula_sum            'C23 H41 K N2 O6'
_chemical_formula_weight         480.68
_chemical_name_common
' (2.2.2-cryptand)-potassium cyclopentadienide '
_chemical_name_systematic
; (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane-\k^8^N~2~,O~6~)
 potassium cyclopentadienide 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.705(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9817(6)
_cell_length_b                   23.8330(15)
_cell_length_c                   9.7379(7)
_cell_measurement_reflns_used    10196
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.6708
_cell_measurement_theta_min      3.0307
_cell_volume                     2540.1(3)
_computing_cell_refinement
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d [1] 
;
_computing_data_collection
; 
 CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.34d [1] 
;
_computing_data_reduction
; 
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d [1] 
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012) [4]'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015) [3]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008) [2]'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'Sapphire 3'
_diffrn_detector_area_resol_mean 16.0238
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Xcalibur 3'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            32316
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.995
_diffrn_reflns_theta_min         3.040
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d 

Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                4029
_reflns_number_total             6125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0296_suppl.cif
_cod_data_source_block           CF-113
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8104580
_shelx_res_checksum              2197
_shelx_hkl_checksum              49646