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_1574199
_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            'C38 H63.5 Mo N5 O0.75 P2 S'
_chemical_formula_weight         792.37
_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.cc2j5klw
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-01-29 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                   31.9495(3)
_cell_length_b                   14.14073(19)
_cell_length_c                   18.9898(2)
_cell_measurement_reflns_used    25190
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.5750
_cell_measurement_theta_min      3.1600
_cell_volume                     8579.39(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65614
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.364
_diffrn_reflns_theta_min         3.125
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.905
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) 
Numerical absorption correction based on gaussian integration over 
a multifaceted crystal model 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       rod
_exptl_crystal_F_000             3364
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8599
_refine_ls_number_restraints     1077
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0445P)^2^+23.6139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7253
_reflns_number_total             8599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00454c3.cif
_cod_data_source_block           SM-647a_Pcca_faces
_cod_depositor_comments
'Adding full bibliography for 1574195--1574200.cif.'
_cod_original_formula_sum        'C38 H63.50 Mo N5 O0.75 P2 S'
_cod_database_code               1574199
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.454
_shelx_estimated_absorpt_t_max   0.926
_shelx_res_checksum              39898