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_1566578
_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
'C32 H12 B F24, C20 H50 Cl N3 P2 Re, 0.5(O C4 H10)'
_chemical_formula_sum            'C54 H67 B Cl F24 N3 O0.5 P2 Re'
_chemical_formula_weight         1516.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                92.777(3)
_cell_angle_beta                 109.357(4)
_cell_angle_gamma                97.022(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2681(5)
_cell_length_b                   15.3208(6)
_cell_length_c                   17.9247(8)
_cell_measurement_reflns_used    26404
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      65.8470
_cell_measurement_theta_min      2.6070
_cell_volume                     3140.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (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 22.2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1340
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            109426
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.597
_diffrn_reflns_theta_min         2.625
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    5.653
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1518
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.890
_refine_diff_density_min         -1.947
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     928
_refine_ls_number_reflns         10946
_refine_ls_number_restraints     295
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0619P)^2^+3.6271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8233
_reflns_number_total             10946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04503b2.cif
_cod_data_source_block           007b-17124
_cod_original_formula_sum        'C54 H67 B Cl F24 N3 O0.50 P2 Re'
_cod_database_code               1566578
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.946
_shelx_res_checksum              1165
_shelx_hkl_checksum              22104