Scandium-Promoted Direct Conversion of Dinitrogen into Hydrazine Derivatives via N-C Bond Formation.
Lv, Ze-Jie; Huang, Zhe; Zhang, Wen-Xiong; Xi, Zhenfeng; Journal of the American Chemical Society 141 (2019) 8773–8777; doi:10.1021/jacs.9b04293

data_4127610
_publ_section_title
;
 Scandium-Promoted Direct Conversion of Dinitrogen into Hydrazine
 Derivatives via N-C Bond Formation.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8773
_journal_page_last               8777
_journal_paper_doi               10.1021/jacs.9b04293
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C42 H76 N6 Sc2, C18 H36 K N2 O6'
_chemical_formula_sum            'C60 H112 K N8 O6 Sc2'
_chemical_formula_weight         1170.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                113.865(3)
_cell_angle_beta                 95.582(2)
_cell_angle_gamma                102.815(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6301(3)
_cell_length_b                   16.8287(5)
_cell_length_c                   18.4005(5)
_cell_measurement_reflns_used    26547
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.1000
_cell_measurement_theta_min      3.8240
_cell_volume                     3949.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_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    -31.00   5.00   0.50    8.03    --   -1.70 -82.00   0.00   72
  2  \w    -15.00  29.00   0.50    8.03    --   -1.70 -82.00  60.00   88
  3  \w    -44.00 -18.00   0.50    8.03    --   -1.70 -57.00-150.00   52
  4  \w    -81.00 -55.00   0.50    8.03    --   -1.70 -57.00-150.00   52
  5  \w    -28.00  29.00   0.50    8.03    --   -1.70 -82.00-150.00  114
  6  \w     61.00  91.00   0.50    8.03    --    1.90  38.00  30.00   60
  7  \w    -16.00  47.00   0.50    8.03    --    1.90  38.00  30.00  126
  8  \w    -18.00  88.00   0.50    8.03    --    1.90  57.00-180.00  212
  9  \w    -30.00  11.00   0.50    8.03    --    1.90 -82.00  30.00   82
 10  \w    -19.00  26.00   0.50    8.03    --    1.90 -19.00  30.00   90
 11  \w    -75.00 -50.00   0.50    8.03    --    1.90 -19.00  30.00   50
 12  \w    -22.00   4.00   0.50    8.03    --    1.90 -82.00 150.00   52
;
_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      -0.0014763000
_diffrn_orient_matrix_UB_12      0.0127636000
_diffrn_orient_matrix_UB_13      -0.0323163000
_diffrn_orient_matrix_UB_21      0.0115662000
_diffrn_orient_matrix_UB_22      -0.0397816000
_diffrn_orient_matrix_UB_23      -0.0247959000
_diffrn_orient_matrix_UB_31      -0.0494968000
_diffrn_orient_matrix_UB_32      -0.0238600000
_diffrn_orient_matrix_UB_33      -0.0141187000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72555
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.477
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_description       block
_exptl_crystal_F_000             1274
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         15500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0560P)^2^+0.9135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13238
_reflns_number_total             15500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04293_si_002.cif
_cod_data_source_block           3
_cod_database_code               4127610
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sc C H N O K'
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.958
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=
 Sof(H3BC)=Sof(H3BD)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(H5C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9), C27(H27), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD), C4(H4A,H4B),
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,
 H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
 C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B),
  C59(H59A,H59B), C60(H60A,H60B)
3.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_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 1.528
_oxdiff_exptl_absorpt_empirical_full_min 0.684