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_4517998
_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_moiety         'C49 H72 Mo N5 P4 Rh Si3'
_chemical_formula_sum            'C49 H72 Mo N5 P4 Rh Si3'
_chemical_formula_weight         1138.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.942(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3056(15)
_cell_length_b                   19.7149(15)
_cell_length_c                   13.1491(8)
_cell_measurement_reflns_used    6053
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.63
_cell_volume                     6275.3(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX II v2014.11-0 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
'0.50 degree frames measured for 20 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20837
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.383
_diffrn_reflns_theta_min         1.332
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0628 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.8362.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       plate
_exptl_crystal_F_000             2360
_exptl_crystal_recrystallization_method
'vapor diffusion of pentane into a THF solution'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.305
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5912
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0618
_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/[\s^2^(Fo^2^)+(0.0844P)^2^+66.3368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4169
_reflns_number_total             5912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc0c00944_si_002.cif
_cod_data_source_block           19066mp_sq
_cod_depositor_comments
'Adding full bibliography for 4517996--4518010.cif.'
_cod_database_code               4517998
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.757
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H24A,H24B} of C24, {H29C,H29D} of C29A, {H29A,H29B} of
  C29, {H23A,H23B} of C23, {H8A,H8B} of C8, {H7A,H7B} of C7, All C(H,H,H,H)
  groups
 At 1.5 times of:
  All C(H,H,H) groups, {H22A,H22B} of C22
2. Restrained distances
 N4-C29A \\sim N4-C29
 with sigma of 0.02
 C28-C29A \\sim C28-C29
 with sigma of 0.02
 P1-N1 \\sim N2-P2
 with sigma of 0.02
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(P2) = Uanis(N1)
Uanis(P1) = Uanis(N2)
Uanis(C29A) = Uanis(C29)
5. Others
 Sof(P2)=Sof(N2)=0.5*(1-FVAR(2))
 Sof(P1)=Sof(N1)=0.5*FVAR(2)
 Fixed Sof: C1(0.5) C2(0.5) H2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5)
 H5(0.5) C6(0.5) H6(0.5) H23A(0.5) H23B(0.5) C24(0.5) H24A(0.5) H24B(0.5)
 H28C(0.5) H28D(0.5) H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5) C29A(0.5)
 H29C(0.5) H29D(0.5)
6.a Riding coordinates:
 C22(H22A,H22B)
6.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C23(H23A,H23B), C24(H24A,H24B), C28(H28C,H28D),
 C28(H28A,H28B), C29(H29A,H29B), C29A(H29C,H29D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              7768
_shelx_hkl_checksum              42261
_shelx_fab_checksum              99244
_olex2_submission_special_instructions 'No special instructions were received'