Ammonia synthesis by the reductive N-N bond cleavage of hydrazine using an air-stable, phosphine-free ruthenium catalyst.
Mohanty, Aisa; Rout, Smruti Rekha; Dandela, Rambabu; Daw, Prosenjit; Chemical communications (Cambridge, England) 60 (2024) 416–419; doi:10.1039/d3cc04490d

data_7132587
_publ_section_title
;
 Ammonia synthesis by the reductive N-N bond cleavage of hydrazine using
 an air-stable, phosphine-free ruthenium catalyst.
;
_journal_issue                   4
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              416
_journal_page_last               419
_journal_paper_doi               10.1039/d3cc04490d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(C25 H30 N5),C H2 Cl2'
_chemical_formula_sum            'C25.5 H31 Cl N5'
_chemical_formula_weight         443.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-08-26 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.266(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.863(3)
_cell_length_b                   9.4396(9)
_cell_length_c                   17.2974(16)
_cell_measurement_reflns_used    2027
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      0.971
_cell_measurement_theta_min      0.957
_cell_volume                     4782.1(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 quest photon detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28059
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.107
_diffrn_reflns_theta_max         25.107
_diffrn_reflns_theta_min         2.267
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.129
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.0051(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4252
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+3.4676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.2061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2027
_reflns_number_total             4252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04490d2.cif
_cod_data_source_block           pd_am_l1_0m
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C25.50 H31 Cl N5'
_cod_database_code               7132587
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              27548
_shelx_hkl_checksum              5042