Mechanistic Insights into N-N Bond Cleavage in Catalytic Guanylation Reactions between 1,2-Diarylhydrazines and Carbodiimides.
Xu, Ling; Wang, Yu-Chen; Ma, Wangyang; Zhang, Wen-Xiong; Xi, Zhenfeng; The Journal of organic chemistry 79 (2014) 12004–12009; doi:10.1021/jo501865b

data_4030084
_publ_section_title
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 Mechanistic Insights into N-N Bond Cleavage in Catalytic Guanylation
 Reactions between 1,2-Diarylhydrazines and Carbodiimides.
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_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12004
_journal_page_last               12009
_journal_paper_doi               10.1021/jo501865b
_journal_volume                  79
_journal_year                    2014
_chemical_formula_moiety         'C48 H57 Li3 N6 O3, C6 H14'
_chemical_formula_sum            'C54 H71 Li3 N6 O3'
_chemical_formula_weight         872.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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Olex2 1.2
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_cell_length_b                   13.6874(4)
_cell_length_c                   14.4188(4)
_cell_measurement_reflns_used    8123
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
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_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0509659000
_diffrn_orient_matrix_UB_12      0.0063856000
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_diffrn_orient_matrix_UB_21      0.0101280000
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_diffrn_orient_matrix_UB_23      0.0327231000
_diffrn_orient_matrix_UB_31      0.0192064000
_diffrn_orient_matrix_UB_32      -0.0313178000
_diffrn_orient_matrix_UB_33      0.0407705000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       16
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.881
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.070
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
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_exptl_crystal_colour
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_exptl_crystal_density_diffrn    1.147
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_exptl_crystal_F_000             940
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_refine_ls_number_reflns         9950
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_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0470
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'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.8737P] where P=(Fo^2^+2Fc^2^)/3'
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'Adding full bibliography for 4030083--4030085.cif.'
_cod_database_code               4030084
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_chemical_oxdiff_formula         'C15 N2 H30 Li O'
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_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 Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B),
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2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4A), C5(H5), C6(H6A), C8(H8), C9(H9), C10(H10), C11(H11),
  C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
  C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C54(H54A,H54B,H54C)
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