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_4517874
_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         'C44 H72 Cs2 N2 O4, C4 H8 O'
_chemical_formula_sum            'C48 H80 Cs2 N2 O5'
_chemical_formula_weight         1030.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 104.40(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.16(2)
_cell_length_b                   12.227(4)
_cell_length_c                   21.282(7)
_cell_measurement_reflns_used    26718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.199
_cell_measurement_theta_min      1.943
_cell_volume                     9870(7)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      ' 163 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26718
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         1.943
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_T_max  0.8362
_exptl_absorpt_correction_T_min  0.7333
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       plate
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.1740
_exptl_crystal_size_mid          0.1150
_exptl_crystal_size_min          0.0660
_refine_diff_density_max         0.695
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00059(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         8878
_refine_ls_number_restraints     2939
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+79.0336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7592
_reflns_number_total             8878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02414_si_002.cif
_cod_data_source_block           fe0235_a
_cod_original_cell_volume        9870(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4517874
_shelx_shelxl_version_number     2018/3