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_4127614
_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         'C45 H82 N6 O Sc2'
_chemical_formula_sum            'C45 H82 N6 O Sc2'
_chemical_formula_weight         813.08
_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                 98.785(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3715(2)
_cell_length_b                   32.6101(7)
_cell_length_c                   14.2088(3)
_cell_measurement_reflns_used    22855
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.8390
_cell_measurement_theta_min      3.6180
_cell_volume                     4749.26(17)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -92.00 -67.00   0.50   25.11    --  -10.90  19.00-150.00   50
  2  \w    -34.00  29.00   0.50   25.11    --  -10.90 -77.00 150.00  126
  3  \w     25.00  51.00   0.50   25.11    --  -10.90  19.00-150.00   52
  4  \w    -47.00 -16.00   0.50   25.11    --  -10.90  19.00-150.00   62
  5  \w      1.00  29.00   0.50   25.11    --  -10.90 -82.00-180.00   56
  6  \w    -32.00  -7.00   0.50   25.11    --  -10.90 -82.00-120.00   50
  7  \w    -22.00   3.00   0.50   25.11    --  -10.90 -82.00  30.00   50
  8  \w    -39.00  -6.00   0.50   25.11    --  -10.90 -77.00 120.00   66
  9  \w    -23.00  54.00   0.50   25.11    --   10.90 -82.00  60.00  154
 10  \w    -40.00  39.00   0.50   25.11    --   10.90 -77.00-150.00  158
 11  \w    -26.00  45.00   0.50   25.11    --   10.90 -82.00 -30.00  142
 12  \w    -34.00  32.00   0.50   25.11    --   10.90 -82.00   0.00  132
 13  \w    -52.00  55.00   0.50   25.11    --   10.90 -37.00  60.00  214
;
_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      -0.0207921000
_diffrn_orient_matrix_UB_12      0.0200382000
_diffrn_orient_matrix_UB_13      0.0100303000
_diffrn_orient_matrix_UB_21      -0.0596605000
_diffrn_orient_matrix_UB_22      -0.0081183000
_diffrn_orient_matrix_UB_23      0.0104690000
_diffrn_orient_matrix_UB_31      0.0282411000
_diffrn_orient_matrix_UB_32      -0.0023959000
_diffrn_orient_matrix_UB_33      0.0483791000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72727
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71956
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         9297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0575P)^2^+6.9093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7800
_reflns_number_total             9297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04293_si_002.cif
_cod_data_source_block           12
_cod_database_code               4127614
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Sc C H N O'
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.959
_reflns_odcompleteness_completeness 99.74
_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. Others
 Sof(H33A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(H33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C30(H30), C33(H33), C33(H33A)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F), C35(H35A,H35B,H35C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C)
;
_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 1.387
_oxdiff_exptl_absorpt_empirical_full_min 0.700