Formation and structural characterization of a potassium amidinoguanidinate
Lorenz, Volker; Liebing, Phil; Hilfert, Liane; Busse, Sabine; Edelmann, Frank T.; Acta Crystallographica Section E 74 (2018) 1795–1799; doi:10.1107/S2056989018015980

data_2242740
_publ_section_title
;
 Formation and structural characterization of a potassium
 amidinoguanidinate
;
_journal_coeditor_code           ZL2742
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1795
_journal_page_last               1799
_journal_paper_doi               10.1107/S2056989018015980
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[K2 (C14 H32 N4)2 (C4 H10 O2)]'
_chemical_formula_moiety         'C32 H68 K2 N8 O2'
_chemical_formula_sum            'C32 H68 K2 N8 O2'
_chemical_formula_weight         675.14
_chemical_name_systematic
<i>catena</i>-Poly[[bis(\m-1-amidinato-<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>'''-tetraisopropylguanidinato-\k^5^<i>N</i>^1^:<i>N</i>^1^,<i>N</i>^2^:<i>N</i>^2^,<i>N</i>^4^)dipotassium]-\m-1,2-dimethoxyethane-\k^2^<i>O</i>:<i>O</i>']
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                71.605(4)
_cell_angle_beta                 64.168(4)
_cell_angle_gamma                63.516(4)
_cell_formula_units_Z            1
_cell_length_a                   10.3207(6)
_cell_length_b                   10.5311(6)
_cell_length_c                   11.6703(7)
_cell_measurement_reflns_used    12337
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.175
_cell_measurement_theta_min      1.961
_cell_volume                     1010.23(11)
_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
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR-97 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1042
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9148
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.351
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_description       plate
_exptl_crystal_F_000             370
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.682
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0873P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                3368
_reflns_number_total             3941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2742sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C16 H34 K N4 O'
_cod_original_formula_sum        'C16 H34 K N4 O'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     337.57
_cod_database_code               2242740
_cod_database_fobs_code          2242740
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.958
_shelx_hkl_checksum              71876
_shelx_res_checksum              25593