Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-κ6O6) 1,2,3,4,5-pentamethyl-cyclopenta-2,4-dien-1-yl(potassium, rubidium) — ammonia (1/2), [K0.3Rb0.7(18-crown-6)]Cp*⋅2 NH3, C22H45K0.3N2O6Rb0.7
Henneberger, Thomas; Klein, Wilhelm; Fässler, Thomas F.; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1241–1243; doi:10.1515/ncrs-2019-0368

data_8105993
_publ_section_title
;
 Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-\k6O6)
 1,2,3,4,5-pentamethyl-cyclopenta-2,4-dien-1-yl(potassium, rubidium) ---
 ammonia (1/2), [K0.3Rb0.7(18-crown-6)]Cp*&#x22C5;2 NH3,
 C22H45K0.3N2O6Rb0.7
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1241
_journal_page_last               1243
_journal_paper_doi               10.1515/ncrs-2019-0368
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C22 H39 K0.26 O6 Rb0.74, 2(H3 N)'
_chemical_formula_sum            'C22 H45 K0.26 N2 O6 Rb0.74'
_chemical_formula_weight         506.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.1587(8)
_cell_length_b                   16.2842(15)
_cell_length_c                   32.862(3)
_cell_measurement_reflns_used    3359
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.8069
_cell_measurement_theta_min      3.0001
_cell_volume                     5436.2(8)
_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_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1856
_diffrn_reflns_av_unetI/netI     0.2169
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            57130
_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         25.995
_diffrn_reflns_theta_min         3.007
_exptl_absorpt_coefficient_mu    1.432
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91191
_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            yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             2170
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.692
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.692
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0137P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0616
_reflns_number_gt                1974
_reflns_number_total             5339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0368_suppl.cif
_cod_data_source_block           TH302
_cod_database_code               8105993
_shelx_shelxl_version_number     2014/7