Dinitrogen reduction to ammonia with a pincer-Mo complex: new insights into the mechanism of nitride-to-ammonia conversion
Mandal, Souvik; Zhou, Xiaoguang; Bruch, Quinton J.; Allen, Rachel N.; Giordano, Laurence W.; Walker, Nicholas J. I.; Emge, Thomas J.; Hasanayn, Faraj; Miller, Alexander J. M.; Malakar, Santanu; Goldman, Alan S.; Chemical Science 16 (2025) 7347–7365; doi:10.1039/D5SC00454C

data_1574197
_publ_section_title
;
 Dinitrogen reduction to ammonia with a pincer-Mo complex: new insights
 into the mechanism of nitride-to-ammonia conversion
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              7347
_journal_page_last               7365
_journal_paper_doi               10.1039/D5SC00454C
_journal_volume                  16
_journal_year                    2025
_chemical_formula_sum            'C41 H65.5 Mo N O2 P2 S'
_chemical_formula_weight         794.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_Hall           '-P 2a 2ac'
_space_group_name_H-M_alt        'P c c a'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2jkh7v
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-03-14 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.877(8)
_cell_length_b                   14.204(4)
_cell_length_c                   18.861(5)
_cell_measurement_reflns_used    3880
_cell_measurement_temperature    426(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.20
_cell_volume                     8540(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  SHELXL-2014/7
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      426(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35946
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.194
_diffrn_reflns_theta_max         24.194
_diffrn_reflns_theta_min         1.905
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       needle
_exptl_crystal_F_000             3380
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_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.007
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     841
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1222
_refine_ls_R_factor_gt           0.0913
_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^)+(0.0700P)^2^+44.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5092
_reflns_number_total             6868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00454c3.cif
_cod_data_source_block           dinitrogen_Pcca_final
_cod_depositor_comments
'Adding full bibliography for 1574195--1574200.cif.'
_cod_original_formula_sum        'C41 H65.50 Mo N O2 P2 S'
_cod_database_code               1574197
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              6015