#------------------------------------------------------------------------------
#$Date: 2024-12-06 18:46:44 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296405 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/24/1572427.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1572427
loop_
_publ_author_name
'Queen, Joshua D.'
'Rajabi, Ahmadreza'
'Goudzwaard, Quinn E.'
'Yuan, Qiong'
'Nguyen, Dang Khoa'
'Ziller, Joseph W.'
'Furche, Filipp'
'Xi, Zhenfeng'
'Evans, William J.'
_publ_section_title
;
 Dinitrogen reduction chemistry with scandium provides a complex with two
 side-on (N[double bond, length as m-dash]N)²⁻ ligands bound to
 one metal:
 (C₅Me₅)Sc[(µ-η²:η²-N₂)Sc(C₅Me₅)₂]₂.
;
_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         'C40 H60 N2 Sc2'
_chemical_formula_sum            'C40 H60 N2 Sc2'
_chemical_formula_weight         658.82
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_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            2
_cell_length_a                   10.9904(15)
_cell_length_b                   11.3937(16)
_cell_length_c                   14.908(2)
_cell_measurement_reflns_used    5027
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.25
_cell_volume                     1866.8(4)
_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      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22932
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.538
_diffrn_reflns_theta_min         2.250
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.14(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0458
_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/[σ²(Fo²)+(0.0621P)²+0.6884P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                2511
_reflns_number_total             2836
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc03977g3.cif
_cod_data_source_block           qeg1
_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               1572427
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.963
_exptl_absorpt_special_details
;
Reflections not merged
22932 Corrected reflections written to file qeg1.hkl
Estimated minimum and maximum transmission:  0.6102  0.7461
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r =  0.2000
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sc1 Sc 0.5000 0.5000 0.67686(4) 0.01479(17) Uani 0.95 2 d S T P A 1
Sc2 Sc 0.5000 0.5000 0.6270(8) 0.0063(16) Uiso 0.05 2 d S . P A 2
N1 N 0.5000 0.5000 0.53939(19) 0.0209(5) Uani 1 2 d S T P A 1
C1 C 0.5822(3) 0.6417(3) 0.7881(2) 0.0227(6) Uani 1 1 d . . . . .
C2 C 0.6743(3) 0.5570(3) 0.7728(2) 0.0225(6) Uani 1 1 d . . . . .
C3 C 0.7139(2) 0.5685(2) 0.6828(2) 0.0218(5) Uani 1 1 d . . . . .
C4 C 0.6476(2) 0.6619(2) 0.64275(18) 0.0202(5) Uani 1 1 d . . . . .
C5 C 0.5636(3) 0.7047(2) 0.70687(19) 0.0211(5) Uani 1 1 d . . . . .
C6 C 0.5287(3) 0.6734(3) 0.8779(2) 0.0305(7) Uani 1 1 d . . . . .
H6A H 0.4481 0.7085 0.8692 0.046 Uiso 1 1 calc R U . . .
H6B H 0.5820 0.7298 0.9082 0.046 Uiso 1 1 calc R U . . .
H6C H 0.5211 0.6025 0.9147 0.046 Uiso 1 1 calc R U . . .
C7 C 0.7334(3) 0.4791(3) 0.8419(2) 0.0315(7) Uani 1 1 d . . . . .
H7A H 0.6830 0.4770 0.8961 0.047 Uiso 1 1 calc R U . . .
H7B H 0.8141 0.5101 0.8568 0.047 Uiso 1 1 calc R U . . .
H7C H 0.7417 0.3996 0.8177 0.047 Uiso 1 1 calc R U . . .
C8 C 0.8147(2) 0.4999(4) 0.6390(2) 0.0303(6) Uani 1 1 d . . . . .
H8A H 0.8166 0.4202 0.6637 0.045 Uiso 1 1 calc R U . . .
H8B H 0.8927 0.5387 0.6506 0.045 Uiso 1 1 calc R U . . .
H8C H 0.8005 0.4961 0.5742 0.045 Uiso 1 1 calc R U . . .
C9 C 0.6689(3) 0.7112(3) 0.5502(2) 0.0268(6) Uani 1 1 d . . . . .
H9A H 0.6517 0.6506 0.5053 0.040 Uiso 1 1 calc R U . . .
H9B H 0.7538 0.7364 0.5447 0.040 Uiso 1 1 calc R U . . .
H9C H 0.6150 0.7785 0.5405 0.040 Uiso 1 1 calc R U . . .
C10 C 0.4732(3) 0.8019(3) 0.6932(2) 0.0284(7) Uani 1 1 d . . . . .
H10A H 0.4507 0.8059 0.6297 0.043 Uiso 1 1 calc R U . . .
H10B H 0.5095 0.8766 0.7117 0.043 Uiso 1 1 calc R U . . .
H10C H 0.4004 0.7865 0.7294 0.043 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Sc1 C5 100.42(7) . 2_665 ?
N1 Sc1 C5 100.42(7) . . ?
C5 Sc1 C5 159.17(14) 2_665 . ?
N1 Sc1 C2 125.28(7) . 2_665 ?
C5 Sc1 C2 55.27(10) 2_665 2_665 ?
C5 Sc1 C2 111.15(10) . 2_665 ?
N1 Sc1 C2 125.28(7) . . ?
C5 Sc1 C2 111.16(10) 2_665 . ?
C5 Sc1 C2 55.27(10) . . ?
C2 Sc1 C2 109.44(14) 2_665 . ?
N1 Sc1 C3 92.05(7) . 2_665 ?
C5 Sc1 C3 55.18(9) 2_665 2_665 ?
C5 Sc1 C3 123.92(9) . 2_665 ?
C2 Sc1 C3 33.23(10) 2_665 2_665 ?
C2 Sc1 C3 142.66(10) . 2_665 ?
N1 Sc1 C3 92.05(7) . . ?
C5 Sc1 C3 123.92(9) 2_665 . ?
C5 Sc1 C3 55.18(9) . . ?
C2 Sc1 C3 142.66(10) 2_665 . ?
C2 Sc1 C3 33.23(10) . . ?
C3 Sc1 C3 175.90(15) 2_665 . ?
N1 Sc1 C1 131.88(7) . 2_665 ?
C5 Sc1 C1 33.34(10) 2_665 2_665 ?
C5 Sc1 C1 126.44(10) . 2_665 ?
C2 Sc1 C1 33.16(10) 2_665 2_665 ?
C2 Sc1 C1 93.78(10) . 2_665 ?
C3 Sc1 C1 55.01(10) 2_665 2_665 ?
C3 Sc1 C1 121.71(10) . 2_665 ?
N1 Sc1 C1 131.89(7) . . ?
C5 Sc1 C1 126.44(10) 2_665 . ?
C5 Sc1 C1 33.34(10) . . ?
C2 Sc1 C1 93.77(10) 2_665 . ?
C2 Sc1 C1 33.16(10) . . ?
C3 Sc1 C1 121.71(10) 2_665 . ?
C3 Sc1 C1 55.01(10) . . ?
C1 Sc1 C1 96.23(14) 2_665 . ?
N1 Sc1 C4 78.31(6) . . ?
C5 Sc1 C4 155.77(10) 2_665 . ?
C5 Sc1 C4 33.00(9) . . ?
C2 Sc1 C4 144.09(10) 2_665 . ?
C2 Sc1 C4 54.85(9) . . ?
C3 Sc1 C4 148.46(9) 2_665 . ?
C3 Sc1 C4 33.10(9) . . ?
C1 Sc1 C4 148.01(10) 2_665 . ?
C1 Sc1 C4 54.72(9) . . ?
N1 Sc1 C4 78.31(6) . 2_665 ?
C5 Sc1 C4 33.00(9) 2_665 2_665 ?
C5 Sc1 C4 155.77(10) . 2_665 ?
C2 Sc1 C4 54.85(9) 2_665 2_665 ?
C2 Sc1 C4 144.09(10) . 2_665 ?
C3 Sc1 C4 33.10(9) 2_665 2_665 ?
C3 Sc1 C4 148.46(9) . 2_665 ?
C1 Sc1 C4 54.72(9) 2_665 2_665 ?
C1 Sc1 C4 148.01(10) . 2_665 ?
C4 Sc1 C4 156.61(13) . 2_665 ?
C4 Sc2 C4 169.1(6) . 2_665 ?
C4 Sc2 C3 141.7(3) . 2_665 ?
C4 Sc2 C3 32.32(10) 2_665 2_665 ?
C4 Sc2 C3 32.32(10) . . ?
C4 Sc2 C3 141.7(3) 2_665 . ?
C3 Sc2 C3 142.9(5) 2_665 . ?
C4 Sc2 C5 140.4(4) . 2_665 ?
C4 Sc2 C5 31.30(11) 2_665 2_665 ?
C3 Sc2 C5 51.03(13) 2_665 2_665 ?
C3 Sc2 C5 110.4(3) . 2_665 ?
C4 Sc2 C5 31.30(11) . . ?
C4 Sc2 C5 140.4(4) 2_665 . ?
C3 Sc2 C5 110.4(3) 2_665 . ?
C3 Sc2 C5 51.03(13) . . ?
C5 Sc2 C5 127.9(5) 2_665 . ?
N1 N1 Sc1 180.0 3_656 . ?
C2 C1 C5 108.0(3) . . ?
C2 C1 C6 125.8(3) . . ?
C5 C1 C6 125.4(3) . . ?
C2 C1 Sc1 73.15(16) . . ?
C5 C1 Sc1 72.97(16) . . ?
C6 C1 Sc1 127.4(2) . . ?
C1 C2 C3 108.0(3) . . ?
C1 C2 C7 126.8(3) . . ?
C3 C2 C7 124.7(3) . . ?
C1 C2 Sc1 73.68(16) . . ?
C3 C2 Sc1 73.42(15) . . ?
C7 C2 Sc1 125.0(2) . . ?
C2 C3 C4 108.1(3) . . ?
C2 C3 C8 126.1(3) . . ?
C4 C3 C8 125.7(3) . . ?
C2 C3 Sc1 73.35(16) . . ?
C4 C3 Sc1 74.63(15) . . ?
C8 C3 Sc1 121.3(2) . . ?
C2 C3 Sc2 89.9(3) . . ?
C4 C3 Sc2 68.22(17) . . ?
C8 C3 Sc2 111.7(2) . . ?
C5 C4 C3 108.0(3) . . ?
C5 C4 C9 126.2(3) . . ?
C3 C4 C9 125.7(3) . . ?
C5 C4 Sc2 83.8(3) . . ?
C3 C4 Sc2 79.5(2) . . ?
C9 C4 Sc2 107.0(3) . . ?
C5 C4 Sc1 72.19(15) . . ?
C3 C4 Sc1 72.28(15) . . ?
C9 C4 Sc1 124.01(18) . . ?
C4 C5 C1 107.9(3) . . ?
C4 C5 C10 126.4(3) . . ?
C1 C5 C10 125.6(3) . . ?
C4 C5 Sc1 74.81(15) . . ?
C1 C5 Sc1 73.69(16) . . ?
C10 C5 Sc1 118.93(18) . . ?
C4 C5 Sc2 64.9(2) . . ?
C1 C5 Sc2 88.7(3) . . ?
C10 C5 Sc2 113.9(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sc1 Cnt1 2.172 . ?
Sc1 N1 2.049(3) . ?
Sc1 C5 2.475(3) 2_665 ?
Sc1 C5 2.475(3) . ?
Sc1 C2 2.477(3) 2_665 ?
Sc1 C2 2.477(3) . ?
Sc1 C3 2.478(3) 2_665 ?
Sc1 C3 2.478(3) . ?
Sc1 C1 2.484(3) 2_665 ?
Sc1 C1 2.484(3) . ?
Sc1 C4 2.509(3) . ?
Sc1 C4 2.509(3) 2_665 ?
Sc2 C4 2.468(3) . ?
Sc2 C4 2.468(3) 2_665 ?
Sc2 C3 2.613(5) 2_665 ?
Sc2 C3 2.613(5) . ?
Sc2 C5 2.710(6) 2_665 ?
Sc2 C5 2.710(6) . ?
N1 N1 1.174(6) 3_656 ?
C1 C2 1.416(4) . ?
C1 C5 1.423(4) . ?
C1 C6 1.506(4) . ?
C2 C3 1.417(4) . ?
C2 C7 1.507(4) . ?
C3 C4 1.421(4) . ?
C3 C8 1.505(4) . ?
C4 C5 1.416(4) . ?
C4 C9 1.508(4) . ?
C5 C10 1.501(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 0.8(3) . . . . ?
C6 C1 C2 C3 -169.7(3) . . . . ?
Sc1 C1 C2 C3 65.94(19) . . . . ?
C5 C1 C2 C7 173.0(3) . . . . ?
C6 C1 C2 C7 2.5(5) . . . . ?
Sc1 C1 C2 C7 -121.9(3) . . . . ?
C5 C1 C2 Sc1 -65.15(19) . . . . ?
C6 C1 C2 Sc1 124.3(3) . . . . ?
C1 C2 C3 C4 1.0(3) . . . . ?
C7 C2 C3 C4 -171.4(3) . . . . ?
Sc1 C2 C3 C4 67.14(18) . . . . ?
C1 C2 C3 C8 177.0(3) . . . . ?
C7 C2 C3 C8 4.5(5) . . . . ?
Sc1 C2 C3 C8 -116.9(3) . . . . ?
C1 C2 C3 Sc1 -66.11(19) . . . . ?
C7 C2 C3 Sc1 121.5(3) . . . . ?
C1 C2 C3 Sc2 -66.0(2) . . . . ?
C7 C2 C3 Sc2 121.6(3) . . . . ?
C2 C3 C4 C5 -2.5(3) . . . . ?
C8 C3 C4 C5 -178.4(3) . . . . ?
Sc1 C3 C4 C5 63.83(19) . . . . ?
Sc2 C3 C4 C5 79.9(3) . . . . ?
C2 C3 C4 C9 174.1(3) . . . . ?
C8 C3 C4 C9 -1.8(4) . . . . ?
Sc1 C3 C4 C9 -119.6(3) . . . . ?
Sc2 C3 C4 C9 -103.5(4) . . . . ?
C2 C3 C4 Sc2 -82.4(3) . . . . ?
C8 C3 C4 Sc2 101.7(4) . . . . ?
C2 C3 C4 Sc1 -66.29(18) . . . . ?
C8 C3 C4 Sc1 117.7(3) . . . . ?
C3 C4 C5 C1 2.9(3) . . . . ?
C9 C4 C5 C1 -173.6(3) . . . . ?
Sc2 C4 C5 C1 79.7(3) . . . . ?
Sc1 C4 C5 C1 66.83(19) . . . . ?
C3 C4 C5 C10 -178.9(3) . . . . ?
C9 C4 C5 C10 4.5(4) . . . . ?
Sc2 C4 C5 C10 -102.1(3) . . . . ?
Sc1 C4 C5 C10 -115.0(3) . . . . ?
C3 C4 C5 Sc1 -63.88(18) . . . . ?
C9 C4 C5 Sc1 119.5(3) . . . . ?
C3 C4 C5 Sc2 -76.8(3) . . . . ?
C9 C4 C5 Sc2 106.6(3) . . . . ?
C2 C1 C5 C4 -2.3(3) . . . . ?
C6 C1 C5 C4 168.2(3) . . . . ?
Sc1 C1 C5 C4 -67.58(19) . . . . ?
C2 C1 C5 C10 179.5(3) . . . . ?
C6 C1 C5 C10 -9.9(4) . . . . ?
Sc1 C1 C5 C10 114.2(3) . . . . ?
C2 C1 C5 Sc1 65.27(19) . . . . ?
C6 C1 C5 Sc1 -124.2(3) . . . . ?
C2 C1 C5 Sc2 60.7(2) . . . . ?
C6 C1 C5 Sc2 -128.7(3) . . . . ?
