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_1574198
_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
; 
C35 H57 Cl I Mo N P2 S, (C6 H6) 
;
_chemical_formula_sum            'C41 H63 Cl I Mo N P2 S'
_chemical_formula_weight         922.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2jkh9x
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2024-03-14 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.035(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.017(3)
_cell_length_b                   13.531(3)
_cell_length_c                   18.041(3)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.27
_cell_volume                     4365.1(14)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0694
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31610
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.484
_diffrn_reflns_theta_min         1.886
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  .9999
_exptl_absorpt_correction_T_min  0.8339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .05
_refine_diff_density_max         1.548
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8984
_refine_ls_number_restraints     861
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+19.7989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7397
_reflns_number_total             8984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00454c3.cif
_cod_data_source_block           MoPSPIClNH2_P21c_a
_cod_depositor_comments
'Adding full bibliography for 1574195--1574200.cif.'
_cod_original_cell_volume        4364.9(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1574198
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              25766