Electronic and Spin-State Effects on Dinitrogen Splitting to Nitrides in a Rhenium Pincer System.
Weber, Jeremy E.; Hasanayn, Faraj; Fataftah, Majed; Mercado, Brandon Q.; Crabtree, Robert H.; Holland, Patrick L.; Inorganic chemistry 60 (2021) 6115–6124; doi:10.1021/acs.inorgchem.0c03778

data_4350796
_publ_section_title
;
 Electronic and Spin-State Effects on Dinitrogen Splitting to Nitrides in
 a Rhenium Pincer System.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6115
_journal_page_last               6124
_journal_paper_doi               10.1021/acs.inorgchem.0c03778
_journal_volume                  60
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H42 Cl N2 P2 Re'
_chemical_formula_sum            'C22 H42 Cl N2 P2 Re'
_chemical_formula_weight         618.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8668(3)
_cell_length_b                   14.5601(4)
_cell_length_c                   14.8307(5)
_cell_measurement_reflns_used    28107
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.4640
_cell_measurement_theta_min      2.3480
_cell_volume                     2562.47(13)
_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    'Olex2 (Dolomanov et al., 2009)'
_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 6.8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury275R CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44738
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         3.083
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.982
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66854
_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            Orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       Block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.300
_refine_diff_density_max         2.131
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
; 
 Flack x determined using 2498 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.025(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5886
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0198
_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^)+(0.0151P)^2^+1.1905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5774
_reflns_number_total             5886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic0c03778_si_003.cif
_cod_data_source_block           mini-19049
_cod_database_code               4350796
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.190
_shelx_estimated_absorpt_t_max   0.316
_shelx_res_checksum              24455
_shelx_hkl_checksum              46209