data_js119a
_audit_creation_date               2019-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        staples@chemistry.msu.edu
_audit_contact_author_name         'Staples, R.J.'
_audit_contact_author_phone        517-353-1074
_publ_contact_author_id_orcid      ?
_publ_requested_journal            'Private Communication'
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           '2(H4 N), 4(N1.5)'
_chemical_formula_sum              'H8 N8'
_chemical_formula_weight           120.14
_chemical_melting_point            ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system        'orthorhombic'
_space_group_IT_number             53
_space_group_name_H-M_alt          'P m n a'
_space_group_name_Hall             '-P 2ac 2'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x+1/2, y, -z+1/2'
 'x, -y, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x-1/2, -y, z-1/2'
 '-x, y, z'

_cell_length_a                     8.9331(10)
_cell_length_b                     3.7824(4)
_cell_length_c                     8.6519(10)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       292.34(6)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      3093
_cell_measurement_temperature      173(2)
_cell_measurement_theta_max        27.47
_cell_measurement_theta_min        3.28
_shelx_estimated_absorpt_T_max     0.989
_shelx_estimated_absorpt_T_min     0.970
_exptl_absorpt_coefficient_mu      0.111
_exptl_absorpt_correction_T_max    0.7456
_exptl_absorpt_correction_T_min    0.6885
_exptl_absorpt_correction_type     analytical
_exptl_absorpt_process_details    
 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0510 before and 0.0428 after correction. The Ratio of minimum to maximum transmission is 0.9234. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      1.365
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         'block'
_exptl_crystal_F_000               128
_exptl_crystal_recrystallization_method  'used as received'
_exptl_crystal_size_max            0.273
_exptl_crystal_size_mid            0.184
_exptl_crystal_size_min            0.1
_exptl_special_details            
 'Data was collected using a BRUKER CCD (charge coupled device) based diffractometer equipped with an Oxford low-temperature apparatus operating at 173 K. A suitable crystal was chosen and mounted on a nylon loop using Paratone oil. Data were measured using omega scans of 0.5° per frame for 30 s. The total number of images were based on results from the program COSMO where redundancy was expected to be 4 and completeness to 0.83Α to 100. Cell parameters were retrieved using APEX II software and refined using SAINT on all observed reflections.Data reduction was performed using the SAINT software which corrects for Lp. Scaling and absorption corrections were applied using SADABS6 multi-scan technique, supplied by George Sheldrick. The structure was solved by the direct method using the SHELXT program and refined by least squares method on F2, SHELXL, incorporated in OLEX2.'
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0276
_diffrn_reflns_av_unetI/netI       0.0118
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  1.000
_diffrn_reflns_limit_h_max         11
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         4
_diffrn_reflns_limit_k_min         -4
_diffrn_reflns_limit_l_max         11
_diffrn_reflns_limit_l_min         -11
_diffrn_reflns_number              4901
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  1.000
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.482
_diffrn_reflns_theta_min           3.278
_diffrn_ambient_temperature        173(2)
_diffrn_detector_area_resol_mean   8.36
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  1.000
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         ω
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed tube'
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  318
_reflns_number_total               357
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection         'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction          'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement   
 'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution     
 'SHELXT (Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8)'
_refine_diff_density_max           0.202
_refine_diff_density_min           -0.171
_refine_diff_density_rms           0.044
_refine_ls_extinction_coef         0.16(2)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.179
_refine_ls_hydrogen_treatment      refall
_refine_ls_matrix_type             full
_refine_ls_number_parameters       34
_refine_ls_number_reflns           357
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0284
_refine_ls_R_factor_gt             0.0261
_refine_ls_restrained_S_all        1.179
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0437P)²+0.0246P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0714
_refine_ls_wR_factor_ref           0.0748
_refine_special_details           
 'The structure was refined by Least Squares using version 2014/6 of XL (Sheldrick, 2008) incorporated in Olex2 (Dolomanov et al., 2009). All non-hydrogen atoms were refined anisotropically. Hydrogen atom positions were calculated geometrically and refined using the riding model.'
_olex2_refinement_description
;
;
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 N1 N 0.750000 0.4555(3) 0.250000 0.0203(3) Uani 1 2 d S T P . .
 H1A H 0.7161(10) 0.330(3) 0.3248(11) 0.033(2) Uiso 1 1 d . . . . .
 H1B H 0.6754(11) 0.594(3) 0.2153(10) 0.035(3) Uiso 1 1 d . . . . .
 N2 N 0.63183(10) 0.000000 0.500000 0.0269(3) Uani 1 2 d S T P . .
 N3 N 0.500000 0.000000 0.500000 0.0191(3) Uani 1 4 d S T P . .
 N4 N 0.500000 0.1098(3) 0.87246(10) 0.0257(3) Uani 1 2 d S T P . .
 N5 N 0.500000 0.000000 1.000000 0.0190(3) Uani 1 4 d S T P . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 N1 H1A 0.857(10) . ?
 N1 H1A 0.857(10) 3_655 ?
 N1 H1B 0.899(10) 3_655 ?
 N1 H1B 0.899(10) . ?
 N2 N3 1.1777(9) . ?
 N4 N5 1.1790(8) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 H1A N1 H1A 112.8(14) . 3_655 ?
 H1A N1 H1B 109.3(9) . 3_655 ?
 H1A N1 H1B 108.2(9) . . ?
 H1A N1 H1B 108.2(9) 3_655 3_655 ?
 H1B N1 H1A 109.3(9) . 3_655 ?
 H1B N1 H1B 108.9(13) . 3_655 ?
 N2 N3 N2 180.0 . 5_656 ?
 N4 N5 N4 180.0 . 5_657 ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 N1 H1A N2 0.857(10) 2.103(10) 2.9598(7) 177.0(9) . yes
 N1 H1B N4 0.899(10) 2.071(10) 2.9690(8) 177.0(9) 4_566 yes

_journal_page_last                 2
_journal_volume                    1MSU
_journal_year                      2019
_olex2_diffrn_ambient_temperature_device  'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
 'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id  'JS  Gang Zhao NH5 N3'
_olex2_submission_special_instructions  'No special instructions were received'
