Rubidium and Cesium Enediamide Complexes Derived from Bulky 1,4-Diazadienes
Duraisamy, Ramesh; Liebing, Phil; Harmgarth, Nicole; Lorenz, Volker; Hilfert, Liane; Feneberg, Martin; Goldhahn, Rüdiger; Engelhardt, Felix; Edelmann, Frank T.; ACS Omega  (2020) –; doi:10.1021/acsomega.0c02414

data_4517873
_publ_section_title
;
 Rubidium and Cesium Enediamide Complexes Derived from Bulky
 1,4-Diazadienes
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c02414
_journal_year                    2020
_chemical_formula_moiety         '2(C44 H72 N2 O4 Rb2), C4 H8 O'
_chemical_formula_sum            'C92 H152 N4 O9 Rb4'
_chemical_formula_weight         1800.05
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 105.589(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.5255(7)
_cell_length_b                   12.5779(2)
_cell_length_c                   21.3866(5)
_cell_measurement_reflns_used    49209
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.103
_cell_measurement_theta_min      1.720
_cell_volume                     9463.9(3)
_computing_cell_refinement       'X-Area (STOE & Cie, 2002)'
_computing_data_collection       'X-Area (STOE & Cie, 2002)'
_computing_data_reduction        'X-Area and X-Red (STOE & Cie, 2002)'
_computing_molecular_graphics    'Diamond (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SIR-97 (Altamore et al., 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48333
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.897
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.110
_exptl_absorpt_correction_T_max  0.7552
_exptl_absorpt_correction_T_min  0.5507
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Area and X-Red (STOE & Cie, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       plate
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         16209
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+10.7852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11844
_reflns_number_total             16209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02414_si_002.cif
_cod_data_source_block           li0025
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4517873
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.450
_shelx_estimated_absorpt_t_max   0.757