Solvothermal Synthesis, Crystal Growth, and Structure Determination of Sodium and Potassium Guanidinate
Peter Klaus Sawinski; Richard Dronskowski; Inorganic Chemistry 51 (2012) 7425–7430; doi:10.1021/ic301005x

data_4329661
_publ_contact_author_address
;
Institute of Inorganic Chemistry
RWTH Aachen University     
D-52056 Aachen
Germany
;
_publ_contact_author_email       drons@HAL9000.ac.rwth-aachen.de
_publ_contact_author_fax         00492418092642
_publ_contact_author_name        'Prof Dr. Richard Dronskowski'
_publ_contact_author_phone       00492418093642
_publ_section_title
;
 Solvothermal Synthesis, Crystal Growth, and Structure Determination of
 Sodium and Potassium Guanidinate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7425
_journal_page_last               7430
_journal_paper_doi               10.1021/ic301005x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C H4 K N3'
_chemical_formula_weight         97.17
_chemical_name_systematic
;
 potassium guanidinate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.626(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   7.1200(9)
_cell_length_b                   6.9385(9)
_cell_length_c                   30.404(4)
_cell_measurement_reflns_used    2561
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      3.01
_cell_volume                     1497.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Balls&Sticks(Ozawa, Kang, 2004)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1635
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            17035
_diffrn_reflns_theta_full        26.56
_diffrn_reflns_theta_max         26.56
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  0.9207
_exptl_absorpt_correction_T_min  0.7953
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   PLATON
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3115
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                2594
_reflns_number_total             3115
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic301005x_si_001_2.cif
_cod_data_source_block           KCN3H4
_cod_database_code               4329661