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_4127612
_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 I2 N4 Sc2'
_chemical_formula_sum            'C42 H76 I2 N4 Sc2'
_chemical_formula_weight         980.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 101.269(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6058(2)
_cell_length_b                   13.9131(2)
_cell_length_c                   17.8895(3)
_cell_measurement_reflns_used    21324
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      30.7840
_cell_measurement_theta_min      3.7610
_cell_volume                     2344.77(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  31.00   0.50    1.83    --   -1.70 -82.00  30.00  124
  2  \w    -33.00  18.00   0.50    1.83    --   -1.70 -82.00-150.00  102
  3  \w    -32.00  21.00   0.50    1.83    --   -1.70 -82.00 120.00  106
  4  \w    -24.00   1.00   0.50    1.83    --   -1.70 -82.00-180.00   50
  5  \w      4.00  29.00   0.50    1.83    --   -1.70 -82.00 -90.00   50
  6  \w    -20.00  82.00   0.50    1.83    --   -1.70  57.00 150.00  204
  7  \w    -29.00  34.00   0.50    1.83    --    1.90 -82.00 -30.00  126
  8  \w     20.00  65.00   0.50    1.83    --    1.90  37.00 -30.00   90
  9  \w    -87.00  -2.00   0.50    1.83    --    1.90 -37.00  30.00  170
;
_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      0.0014684000
_diffrn_orient_matrix_UB_12      -0.0037958000
_diffrn_orient_matrix_UB_13      0.0396878000
_diffrn_orient_matrix_UB_21      -0.0749914000
_diffrn_orient_matrix_UB_22      -0.0043296000
_diffrn_orient_matrix_UB_23      -0.0073461000
_diffrn_orient_matrix_UB_31      0.0063057000
_diffrn_orient_matrix_UB_32      -0.0506663000
_diffrn_orient_matrix_UB_33      -0.0023453000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41559
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.641
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0332P)^2^+2.4533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4316
_reflns_number_total             4596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04293_si_002.cif
_cod_data_source_block           7
_cod_database_code               4127612
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sc C H N I'
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.768
_reflns_odcompleteness_completeness 99.68
_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(H3BC)=Sof(H3BD)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C00O)=Sof(H00A)=Sof(H00B)=Sof(C00P)=Sof(H00C)=
 Sof(H00D)=Sof(H00E)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C9(H9), C6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3AA,H3AB), C3(H3BC,H3BD), C00O(H00A,H00B), C4(H4A,H4B)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C10(H10A,H10B,
 H10C), C19(H19A,H19B,H19C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C21(H21A,H21B,
 H21C), C20(H20A,H20B,H20C), C00P(H00C,H00D,H00E), C5(H5A,H5B,H5C)
;
_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 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.875