Stabilization of the Dinitrogen Analogue, Phosphorus Nitride.
Martinez, Jorge L.; Lutz, Sean A.; Beagan, Daniel M.; Gao, Xinfeng; Pink, Maren; Chen, Chun-Hsing; Carta, Veronica; Moënne-Loccoz, Pierre; Smith, Jeremy M.; ACS central science 6 (2020) 1572–1577; doi:10.1021/acscentsci.0c00944

data_4518008
_publ_section_title
;
 Stabilization of the Dinitrogen Analogue, Phosphorus Nitride.
;
_journal_issue                   9
_journal_name_full               'ACS central science'
_journal_page_first              1572
_journal_page_last               1577
_journal_paper_doi               10.1021/acscentsci.0c00944
_journal_volume                  6
_journal_year                    2020
_chemical_formula_sum            'C75.04 H144.15 B Fe Mo N14 O0.46 P Si3'
_chemical_formula_weight         1527.87
_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_method           SHELXL-2017/1
_cell_angle_alpha                90.5570(10)
_cell_angle_beta                 102.3710(10)
_cell_angle_gamma                114.5830(10)
_cell_formula_units_Z            2
_cell_length_a                   15.5984(7)
_cell_length_b                   15.7039(7)
_cell_length_c                   20.2878(10)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      2.46
_cell_volume                     4386.8(4)
_computing_cell_refinement       'SAINT V8.38A (BrukerNano, 2017)'
_computing_data_collection       'BIS v6.2.9 (BrukerNano, 2018)'
_computing_data_reduction        'SAINT V8.38A (BrukerNano, 2017)'
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_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'0.50 degree frames measured for 2 seconds each'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1259
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            140576
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_min         1.034
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2018'
_exptl_crystal_colour            orange
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_exptl_crystal_description       block
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.610
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         20167
_refine_ls_number_restraints     1096
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2369
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12547
_reflns_number_total             20167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc0c00944_si_002.cif
_cod_data_source_block           64_5
_cod_depositor_comments
'Adding full bibliography for 4517996--4518010.cif.'
_cod_database_code               4518008
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.960
_shelx_res_checksum              57258
_shelx_hkl_checksum              49563