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_4127611
_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         'C44 H82 N6 Sc2'
_chemical_formula_sum            'C44 H82 N6 Sc2'
_chemical_formula_weight         785.07
_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
_atom_sites_solution_primary     dual
_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                77.391(2)
_cell_angle_beta                 89.362(2)
_cell_angle_gamma                89.452(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5267(2)
_cell_length_b                   13.7143(3)
_cell_length_c                   14.9888(3)
_cell_measurement_reflns_used    12964
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.5250
_cell_measurement_theta_min      3.8420
_cell_volume                     2312.09(8)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -33.00  25.00   0.50    2.83    --   -1.70 -82.00  90.00  116
  2  \w    -44.00  19.00   0.50    2.83    --   -1.70 -77.00 150.00  126
  3  \w    -20.00  25.00   0.50    2.83    --   -1.70 -82.00 -60.00   90
  4  \w    -33.00  28.00   0.50    2.83    --   -1.70 -82.00-120.00  122
  5  \w    -20.00   7.00   0.50    2.83    --   -1.70 -77.00  30.00   54
  6  \w    -13.00  16.00   0.50    2.83    --    1.90 -38.00 -90.00   58
  7  \w    -88.00 -34.00   0.50    2.83    --    1.90 -38.00 -90.00  108
  8  \w    -46.00  29.00   0.50    2.83    --    1.90 -77.00   0.00  150
;
_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      -0.0448499000
_diffrn_orient_matrix_UB_12      0.0228506000
_diffrn_orient_matrix_UB_13      -0.0295555000
_diffrn_orient_matrix_UB_21      0.0086286000
_diffrn_orient_matrix_UB_22      -0.0357592000
_diffrn_orient_matrix_UB_23      -0.0272674000
_diffrn_orient_matrix_UB_31      -0.0412471000
_diffrn_orient_matrix_UB_32      -0.0317496000
_diffrn_orient_matrix_UB_33      0.0271036000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33309
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.614
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80683
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0477P)^2^+0.5950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7815
_reflns_number_total             9082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04293_si_002.cif
_cod_data_source_block           4
_cod_database_code               4127611
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sc C H N O K'
_chemical_oxdiff_usercomment     'zyh180501g, epeN4Mg'
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.962
_reflns_odcompleteness_completeness 99.47
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C29(H29), C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
;
_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 1.348
_oxdiff_exptl_absorpt_empirical_full_min 0.703