Catalytic NH<sub>3</sub> oxidation to N<sub>2</sub> by hydrogen atom abstraction using a low-valent molybdenum complex.
Benedict, Rory J.; Heiden, Zachariah M.; Stephens, David N.; Arulsamy, Navamoney; Mock, Michael T.; Chemical communications (Cambridge, England) 61 (2025) 10315–10318; doi:10.1039/d5cc02433a

data_7134648
_publ_section_title
;
 Catalytic NH<sub>3</sub> oxidation to N<sub>2</sub> by hydrogen atom
 abstraction using a low-valent molybdenum complex.
;
_journal_issue                   56
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10315
_journal_page_last               10318
_journal_paper_doi               10.1039/d5cc02433a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C29 H39 Mo N3 O3 P2'
_chemical_formula_sum            'C29 H39 Mo N3 O3 P2'
_chemical_formula_weight         635.51
_chemical_name_common            DS-Mo1
_chemical_name_systematic        Mo(CO)3(MeCN)(P2N2)
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2025-03-16 deposited with the CCDC.	2025-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.628(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2585(15)
_cell_length_b                   21.027(3)
_cell_length_c                   11.8947(14)
_cell_measurement_reflns_used    9609
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      34.8877
_cell_measurement_theta_min      3.3690
_cell_volume                     2991.8(7)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1380)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            63691
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_min         1.94
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.686
_exptl_crystal_size_mid          0.423
_exptl_crystal_size_min          0.276
_refine_diff_density_max         1.726
_refine_diff_density_min         -0.918
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         11733
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0427P)^2^+4.5200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                11407
_reflns_number_total             11733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02433a2.cif
_cod_data_source_block           mm132
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134648--7134649.cif.
;
_cod_original_cell_volume        2991.8(6)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7134648
_shelx_res_checksum              80423
_shelx_hkl_checksum              86780