Facile conversion of ammonia to a nitride in a rhenium system that cleaves dinitrogen
Connor, Gannon P.; Delony, Daniel; Weber, Jeremy E.; Mercado, Brandon Q.; Curley, Julia B.; Schneider, Sven; Mayer, James M.; Holland, Patrick L.; Chemical Science  (2022) –; doi:10.1039/D1SC04503B

data_1566577
_publ_section_title
;
 Facile conversion of ammonia to a nitride in a rhenium system that
 cleaves dinitrogen
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04503B
_journal_year                    2022
_chemical_formula_moiety         'C20 H46 Cl N2 P2 Re'
_chemical_formula_sum            'C20 H46 Cl N2 P2 Re'
_chemical_formula_weight         598.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-08-02 deposited with the CCDC.	2022-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.515(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5852(3)
_cell_length_b                   23.5810(7)
_cell_length_c                   12.2292(4)
_cell_measurement_reflns_used    10397
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.6490
_cell_measurement_theta_min      3.0580
_cell_volume                     2473.39(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_molecular_graphics
; 
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program 
(2009). J. Appl. Cryst., 42, 339-341. 
;
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Dectris Pilatus 3R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35252
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.937
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    5.158
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.871
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5656
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0182P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4806
_reflns_number_total             5656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04503b2.cif
_cod_data_source_block           007c-17049
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1566577
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.425
_shelx_estimated_absorpt_t_max   0.782
_shelx_res_checksum              5639
_shelx_hkl_checksum              46142