Synthesis and Theoretical Characterization of an Acetylene-Ammonia Cocrystal
Roland Boese; Dieter Bläser; Georg Jansen; Journal of the American Chemical Society 131 (2009) 2104–2106; doi:10.1021/ja8059705

data_4103898
_publ_contact_author
;
         Prof. Dr. Boese, Roland
         Fachbereich Chemie der
         Universit\"at Duisburg-Essen
         Campus Essen Universit\"atsstr. 3-5
         D-45117 Essen, Germany
;
_publ_contact_author_email       roland.boese@.uni-due.de
_publ_contact_author_fax         '++49 (0)201 183 2535'
_publ_contact_author_phone       '++49 (0)201 183 2416'
_publ_section_title
;
 Synthesis and Theoretical Characterization of an Acetylene-Ammonia
 Cocrystal
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2104
_journal_page_last               2106
_journal_paper_doi               10.1021/ja8059705
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C2 H5 N'
_chemical_formula_weight         43.07
_chemical_name_systematic
; 
 ammonia acetylene cocrystal 
;
_space_group_IT_number           46
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2a'
_symmetry_space_group_name_H-M   'I m a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.142(4)
_cell_length_b                   6.370(3)
_cell_length_c                   5.889(3)
_cell_measurement_reflns_used    177
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      4.02
_cell_volume                     342.9(3)
_computing_cell_refinement       'BRUKER AXS SMART APEX 2 Vers. 1.0-27'
_computing_data_collection       'BRUKER AXS SMART APEX 2 Vers. 1.0-27'
_computing_data_reduction        'BRUKER AXS SMART APEX 2 Vers. 1.0-27'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2001 / Vers.6.12'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2001 / Vers.6.12'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2001 / Vers.6.12'
_computing_structure_solution    'BRUKER AXS SHELXTL (c) 2001 / Vers.6.12'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type
; 
 Siemens SMART three axis goniometer with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2 / COSMO
 with chi = 0
;
_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  0.0107
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            659
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylindric
_exptl_crystal_F_000             96
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.124
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment
;
 Riding model with idealized hydrogen
 geometries (linear for acetylene, 
 tetrahedral for ammonia) with free 
 isotropic displacement parameters
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     20
_refine_ls_number_reflns         282
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.285
_refine_ls_shift/su_mean         0.059
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1179P)^2^+0.0591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1452
_reflns_number_gt                244
_reflns_number_total             282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8059705_si_002.cif
_cod_data_source_block           amaxdb-ideal
_cod_original_formula_sum        'C2 H2 N H3'
_cod_database_code               4103898