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_4517872
_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         'C32 H51 Cs2 N2 O3'
_chemical_formula_sum            'C32 H51 Cs2 N2 O3'
_chemical_formula_weight         777.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                64.885(4)
_cell_angle_beta                 85.879(5)
_cell_angle_gamma                69.433(5)
_cell_formula_units_Z            2
_cell_length_a                   11.0782(7)
_cell_length_b                   13.4018(8)
_cell_length_c                   13.8529(8)
_cell_measurement_reflns_used    20376
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.166
_cell_measurement_theta_min      1.972
_cell_volume                     1736.3(2)
_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, 1997)'
_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      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15109
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.144
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.131
_exptl_absorpt_correction_T_max  0.7697
_exptl_absorpt_correction_T_min  0.6066
_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    1.487
_exptl_crystal_description       rod
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6806
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0307P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5688
_reflns_number_total             6806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02414_si_002.cif
_cod_data_source_block           li0231
_cod_database_code               4517872
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.523
_shelx_estimated_absorpt_t_max   0.755