Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-κ 6O6)potassium(2-methylphenylamino)ethyl-2-methylphenylamide ammoniate (1/3.5), [K(18-crown-6)](o-CH3C6H4)NH(CH2)2N(o-CH3C6H4) 3.5 NH3, C28H53.5KN5.5O6
Wallach, Christoph; Klein, Wilhelm; Fässler, Thomas F.; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 897–901; doi:10.1515/ncrs-2022-0275

data_8107246
_publ_section_title
;
 Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-\k
 6O6)potassium(2-methylphenylamino)ethyl-2-methylphenylamide ammoniate
 (1/3.5), [K(18-crown-6)](o-CH3C6H4)NH(CH2)2N(o-CH3C6H4) 3.5 NH3,
 C28H53.5KN5.5O6
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              897
_journal_page_last               901
_journal_paper_doi               10.1515/ncrs-2022-0275
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C12 H30 K N2 O6, C16 H19 N2, 1.5(H3 N)'
_chemical_formula_sum            'C28 H53.5 K N5.5 O6'
_chemical_formula_weight         602.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.554(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7986(12)
_cell_length_b                   8.3431(6)
_cell_length_c                   22.4638(16)
_cell_measurement_reflns_used    167915
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.67
_cell_measurement_theta_min      2.61
_cell_volume                     3463.6(4)
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_collection       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_molecular_graphics    'DIAMOND 3.2k'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40821
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.767
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       sphere
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 3838 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.10(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         13144
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0712
_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^)+(0.1183P)^2^+3.7292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.2226
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.936
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                10077
_reflns_number_total             13144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0275_suppl.cif
_cod_data_source_block           CW-426_Pl_w
_cod_depositor_comments
;

2025-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C56 H107 K2 N11 O12'
_cod_original_formula_weight         1204.72
_cod_original_formula_moiety
'C12 H30 K N2 O6, C12 H27 K N O6, 2(C16 H19 N2), 4(H3 N)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               8107246
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              89153
_shelx_hkl_checksum              56238