Characterization of the Thermally Induced Topochemical Solid-State Transformation of NH4[N(CN)2] into NCNC(NH2)2 by Means of X-ray and Neutron Diffraction as Well as Raman and Solid-State NMR Spectroscopy
Bettina V. Lotsch; Jürgen Senker; Wolfgang Schnick; Inorganic Chemistry 43 (2004) 895–904; doi:10.1021/ic034984f

data_4310538
_publ_contact_author_email       wolfgang.schnick@uni-muenchen.de
_publ_contact_author_fax         089/2180-77440
_publ_contact_author_name        W.Schnick
_publ_section_title
;
 Characterization of the Thermally Induced Topochemical Solid-State
 Transformation of NH4[N(CN)2] into NCNC(NH2)2 by Means of X-ray and
 Neutron Diffraction as Well as Raman and Solid-State NMR Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              895
_journal_page_last               904
_journal_paper_doi               10.1021/ic034984f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C2 H4 N4'
_chemical_formula_weight         84.09
_chemical_name_common            'ammonium dicyanamide'
_chemical_name_systematic        'ammonium dicyanamide'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 91.49(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   3.7913(8)
_cell_length_b                   12.4117(18)
_cell_length_c                   9.1125(13)
_cell_measurement_reflns_used    128
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      35
_cell_measurement_theta_min      5
_cell_volume                     428.66(13)
_computing_data_reduction        'X-Red (Stoe, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE Stadi4'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1923
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_time  1h
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             176
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.048(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.0495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                774
_reflns_number_total             979
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034984fsi20030819_115411.cif
_cod_data_source_block           p:\krist\200k\bl4ek17
_cod_original_cell_volume        428.66(12)
_cod_database_code               4310538