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_1572426
_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         'C34 H53 I N2 O Sc2, C6 H14'
_chemical_formula_sum            'C40 H67 I N2 O Sc2'
_chemical_formula_weight         808.77
_chemical_properties_physical    Air-sensitive
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-05-10 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                   13.4651(9)
_cell_length_b                   14.9197(10)
_cell_length_c                   20.5495(13)
_cell_measurement_reflns_used    9677
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.24
_cell_measurement_theta_min      2.27
_cell_volume                     4128.3(5)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66705
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.624
_diffrn_reflns_theta_min         1.808
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.188
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.5910
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
; 
 Flack x determined using 4921 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.012(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         12559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0537P)^2^+0.3480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                11609
_reflns_number_total             12559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03977g3.cif
_cod_data_source_block           qeg2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1572423--1572428.cif.
;
_cod_database_code               1572426
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.819
_exptl_absorpt_special_details
; 
Reflections not merged 
66828 Corrected reflections written to file qeg2.hkl 
Estimated minimum and maximum transmission:  0.5910  0.7461 
The ratio of these values is more reliable than their absolute values! 
Additional spherical absorption correction applied with mu*r =  0.2000 
;
_shelx_res_checksum              11343
_shelx_hkl_checksum              71132