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_4517871
_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         'C30 H44 N2 O Rb2'
_chemical_formula_sum            'C30 H44 N2 O Rb2'
_chemical_formula_weight         619.61
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 104.0550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.20320(10)
_cell_length_b                   17.71080(10)
_cell_length_c                   13.35680(10)
_cell_measurement_reflns_used    59198
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.5250
_cell_measurement_theta_min      4.2080
_cell_volume                     3029.84(4)
_computing_cell_refinement       'CrysAlisPro (Agilent Tech., 2013)'
_computing_data_collection       'CrysAlisPro (Agilent Tech., 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Tech., 2013)'
_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    'ShelXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            94285
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.992
_diffrn_reflns_theta_min         4.223
_diffrn_source                   'Nova Cu X-ray Source'
_exptl_absorpt_coefficient_mu    4.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro (Agilent Tech., 2013)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       prism
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0327P)^2^+2.0131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5938
_reflns_number_total             6244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c02414_si_002.cif
_cod_data_source_block           magd75
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4517871
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.623
_shelx_estimated_absorpt_t_max   0.845