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_1574195
_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_moiety
; 
 C38 H56 Mo O3 P2 S, 0.5(C5 H12) 
;
_chemical_formula_sum            'C40.5 H61 Mo O3 P2 S'
_chemical_formula_weight         785.83
_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_block_doi                 10.5517/ccdc.csd.cc2gjxc9
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-07-09 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                93.254(2)
_cell_angle_beta                 103.495(2)
_cell_angle_gamma                105.235(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6654(9)
_cell_length_b                   19.2138(15)
_cell_length_c                   19.8632(16)
_cell_measurement_reflns_used    7030
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.33
_cell_volume                     4143.8(6)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.981
_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  0.0567
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47937
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         1.435
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.001
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.539
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         22826
_refine_ls_number_restraints     2071
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0566P)^2^+2.2386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17769
_reflns_number_total             22826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00454c3.cif
_cod_data_source_block           mopspco_P-1_FINAL
_cod_depositor_comments
'Adding full bibliography for 1574195--1574200.cif.'
_cod_original_formula_sum        'C40.50 H61 Mo O3 P2 S'
_cod_database_code               1574195
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              84540