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_1572424
_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         'C24 H38 Cl O Sc'
_chemical_formula_sum            'C24 H38 Cl O Sc'
_chemical_formula_weight         422.95
_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     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                63.797(3)
_cell_angle_beta                 88.175(2)
_cell_angle_gamma                87.697(2)
_cell_formula_units_Z            4
_cell_length_a                   8.4652(3)
_cell_length_b                   16.6864(5)
_cell_length_c                   17.8292(6)
_cell_measurement_reflns_used    19874
_cell_measurement_temperature    179.99(10)
_cell_measurement_theta_max      30.1540
_cell_measurement_theta_min      2.7410
_cell_volume                     2257.53(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.881
_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    -67.00  32.00   0.50    8.00    --   -5.80 -82.00   0.00  198
  2  \w     -1.00  44.00   0.50    8.00    --   -5.80  61.00  79.60   90
  3  \w    -94.00 -67.00   0.50    8.00    --   -5.80 -82.00-150.00   54
  4  \w    -35.00  10.00   0.50    8.00    --   -5.80 -82.00-150.00   90
  5  \w    -31.00  15.00   0.50    8.00    --   -5.80  77.00  30.00   92
  6  \w     24.00  50.00   0.50    8.00    --   -5.80  77.00  30.00   52
  7  \w    -29.00  83.00   0.50    8.00    --   -5.80  57.00-180.00  224
  8  \w    -25.00  68.00   0.50    8.00    --   -5.80  57.00 120.00  186
  9  \w    -10.00  85.00   0.50    8.00    --    5.80  38.00 -30.00  190
;
_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      0.0209489000
_diffrn_orient_matrix_UB_12      -0.0461650000
_diffrn_orient_matrix_UB_13      0.0168835000
_diffrn_orient_matrix_UB_21      0.0483619000
_diffrn_orient_matrix_UB_22      0.0080975000
_diffrn_orient_matrix_UB_23      -0.0357103000
_diffrn_orient_matrix_UB_31      0.0652393000
_diffrn_orient_matrix_UB_32      0.0070460000
_diffrn_orient_matrix_UB_33      0.0201545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46095
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.136
_diffrn_reflns_theta_min         2.236
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0090(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         11733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.7797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9830
_reflns_number_total             11733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03977g3.cif
_cod_data_source_block           1-reducted
_cod_depositor_comments
'Adding full bibliography for 1572423--1572428.cif.'
_cod_database_code               1572424
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C24 H38 O Sc Cl'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C48(H48A,H48B), C24(H24A,H24B), C22(H22A,H22B), C23(H23A,
 H23B), C45(H45A,H45B), C47(H47A,H47B), C46(H46A,H46B)
2.b Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C6(H6A,H6B,H6C), C32(H32A,H32B,H32C), C10(H10A,H10B,
 H10C), C9(H9A,H9B,H9C), C41(H41A,H41B,H41C), C7(H7A,H7B,H7C), C18(H18A,H18B,
 H18C), C42(H42A,H42B,H42C), C31(H31A,H31B,H31C), C8(H8A,H8B,H8C), C016(H01A,
 H01B,H01C), C40(H40A,H40B,H40C), C33(H33A,H33B,H33C), C20(H20A,H20B,H20C),
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C), C34(H34A,H34B,
 H34C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              83674
_shelx_hkl_checksum              5657
_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 1.569
_oxdiff_exptl_absorpt_empirical_full_min 0.636