Dinitrogen reduction chemistry with scandium provides a complex with two side-on (N[double bond, length as m-dash]N)<sup>2-</sup> ligands bound to one metal: (C<sub>5</sub>Me<sub>5</sub>)Sc[(µ-η<sup>2</sup>:η<sup>2</sup>-N<sub>2</sub>)Sc(C<sub>5</sub>Me<sub>5</sub>)<sub>2</sub>]<sub>2</sub>.
Queen, Joshua D.; Rajabi, Ahmadreza; Goudzwaard, Quinn E.; Yuan, Qiong; Nguyen, Dang Khoa; Ziller, Joseph W.; Furche, Filipp; Xi, Zhenfeng; Evans, William J.; Chemical science 15 (2024) 16069–16078; doi:10.1039/d4sc03977g

data_1572428
_publ_section_title
;
 Dinitrogen reduction chemistry with scandium provides a complex with two
 side-on (N[double bond, length as m-dash]N)<sup>2-</sup> ligands bound to
 one metal:
 (C<sub>5</sub>Me<sub>5</sub>)Sc[(&#xb5;-&#x3b7;<sup>2</sup>:&#x3b7;<sup>2</sup>-N<sub>2</sub>)Sc(C<sub>5</sub>Me<sub>5</sub>)<sub>2</sub>]<sub>2</sub>.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              16069
_journal_page_last               16078
_journal_paper_doi               10.1039/d4sc03977g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C20 H30 Cl Sc'
_chemical_formula_sum            'C20 H30 Cl Sc'
_chemical_formula_weight         350.85
_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     dual
_audit_creation_date             2024-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-01 deposited with the CCDC.	2024-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3930(5)
_cell_length_b                   11.1477(7)
_cell_length_c                   20.9045(11)
_cell_measurement_reflns_used    3928
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.1090
_cell_measurement_theta_min      3.1990
_cell_volume                     1955.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     46.00  84.00   0.50    1.50    --   -5.80  38.00 150.00   76
  2  \w    -27.00  27.00   0.50    1.50    --   -5.80  19.00 120.00  108
  3  \w     42.00  77.00   0.50    1.50    --   -5.80  19.00 120.00   70
  4  \w    -16.00  32.00   0.50    1.50    --   -5.80  38.00 150.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0611048000
_diffrn_orient_matrix_UB_12      0.0361677000
_diffrn_orient_matrix_UB_13      -0.0132604000
_diffrn_orient_matrix_UB_21      -0.0570619000
_diffrn_orient_matrix_UB_22      -0.0296900000
_diffrn_orient_matrix_UB_23      0.0193902000
_diffrn_orient_matrix_UB_31      0.0120990000
_diffrn_orient_matrix_UB_32      0.0431568000
_diffrn_orient_matrix_UB_33      0.0244838000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11658
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.890
_diffrn_reflns_theta_min         2.070
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 1478 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0600P)^2^+0.3658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.621
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.733
_reflns_number_gt                4160
_reflns_number_total             4703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03977g3.cif
_cod_data_source_block           1-redcuted
_cod_depositor_comments
'Adding full bibliography for 1572423--1572428.cif.'
_cod_database_code               1572428
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C20 H30 Sc Cl'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C),
 C20(H20A,H20B,H20C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C),
  C17(H17A,H17B,H17C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              52837
_shelx_hkl_checksum              3041
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.135
_oxdiff_exptl_absorpt_empirical_full_min 0.900