Synthesis and Characterization of cyclo-Pentazolate Salts of NH<sub>4</sub><sup>+</sup>, NH<sub>3</sub>OH<sup>+</sup>, N<sub>2</sub>H<sub>5</sub><sup>+</sup>, C(NH<sub>2</sub>)<sub>3</sub><sup>+</sup>, and N(CH<sub>3</sub>)<sub>4</sub><sup/>.
Yang, Chen; Zhang, Chong; Zheng, Zhansheng; Jiang, Chao; Luo, Jun; Du, Yang; Hu, Bingcheng; Sun, Chengguo; Christe, Karl O.; Journal of the American Chemical Society 140 (2018) 16488–16494; doi:10.1021/jacs.8b05106

data_4132610
_publ_section_title
;
 Synthesis and Characterization of cyclo-Pentazolate Salts of
 NH<sub>4</sub><sup>+</sup>, NH<sub>3</sub>OH<sup>+</sup>,
 N<sub>2</sub>H<sub>5</sub><sup>+</sup>,
 C(NH<sub>2</sub>)<sub>3</sub><sup>+</sup>, and
 N(CH<sub>3</sub>)<sub>4</sub><sup/>.
;
_journal_issue                   48
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16488
_journal_page_last               16494
_journal_paper_doi               10.1021/jacs.8b05106
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C72 H60 Ag2 N6 P4'
_chemical_formula_sum            'C72 H60 Ag2 N6 P4'
_chemical_formula_weight         1348.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                114.292(2)
_cell_angle_beta                 101.059(2)
_cell_angle_gamma                90.719(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9399(6)
_cell_length_b                   13.1293(7)
_cell_length_c                   13.1412(7)
_cell_measurement_reflns_used    5699
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.42
_cell_volume                     1526.07(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13853
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.647
_diffrn_reflns_theta_min         2.420
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0144P)^2^+1.0497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5678
_reflns_number_total             7056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            (PPh3)2Ag(N3)2Ag(PPh3)2.cif
_cod_data_source_block           20170710nlg_0m_a
_cod_database_code               4132610
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.820
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
;
_shelx_res_checksum              44568
_shelx_hkl_checksum              33408
_olex2_submission_special_instructions 'No special instructions were received'