Crystal structure of [(1,2-η)-1,2,3,4,5-pentamethyl-cyclopenta-2,4-dien-1-yl] (1,4,10,13-tetraoxa-7,16-diazacyclooctadecane-κ6 N 2,O 4) rubidium (I), [Rb(diaza-18-crown-6)]Cp*, C22H41N2O4Rb
Henneberger, Thomas; Klein, Wilhelm; Fässler, Thomas F.; Zeitschrift für Kristallographie - New Crystal Structures 234 (2018) 165–167; doi:10.1515/ncrs-2018-0252

data_8105576
_publ_section_title
;
 Crystal structure of
 [(1,2-\h)-1,2,3,4,5-pentamethyl-cyclopenta-2,4-dien-1-yl]
 (1,4,10,13-tetraoxa-7,16-diazacyclooctadecane-\k6 N 2,O 4) rubidium (I),
 [Rb(diaza-18-crown-6)]Cp*, C22H41N2O4Rb
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              165
_journal_page_last               167
_journal_paper_doi               10.1515/ncrs-2018-0252
_journal_volume                  234
_journal_year                    2018
_chemical_formula_moiety         'C22 H41 N2 O4 Rb'
_chemical_formula_sum            'C22 H41 N2 O4 Rb'
_chemical_formula_weight         483.04
_chemical_name_systematic
; (1,4,10,13-Tetraoxa-7,16-diazacyclooctadecane-\k^6^N~2~,O~4~) rubidium
 1,2,3,4,5-pentamethyl-cyclopentadienide 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 93.961(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8160(9)
_cell_length_b                   17.7253(16)
_cell_length_c                   13.2179(12)
_cell_measurement_reflns_used    4662
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.8480
_cell_measurement_theta_min      2.9743
_cell_volume                     2528.0(4)
_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 0.998
_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  0.0998
_diffrn_reflns_av_unetI/netI     0.1572
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26792
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.974
_exptl_absorpt_coefficient_mu    1.985
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d [1] 
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.718
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.718
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0273P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                2435
_reflns_number_total             4963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0252_suppl.cif
_cod_data_source_block           TH301
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8105576
_shelx_shelxl_version_number     2014/7