Cu(II)-Catalyzed Oxidative Formation of 5,5'-Bistriazoles.
Brassard, Christopher J.; Zhang, Xiaoguang; Brewer, Christopher R.; Liu, Peiye; Clark, Ronald J.; Zhu, Lei; The Journal of organic chemistry 81 (2016) 12091–12105; doi:10.1021/acs.joc.6b01907

data_4037278
_publ_section_title
;
 Cu(II)-Catalyzed Oxidative Formation of 5,5'-Bistriazoles.
;
_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12091
_journal_page_last               12105
_journal_paper_doi               10.1021/acs.joc.6b01907
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C44 H44 N12, O0.24'
_chemical_formula_sum            'C44 H44 N12 O0.24'
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_space_group_crystal_system      monoclinic
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_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
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_cell_angle_beta                 101.68(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   32.520(15)
_cell_length_c                   9.330(4)
_cell_measurement_reflns_used    1262
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      18.59
_cell_measurement_theta_min      2.51
_cell_volume                     3832(3)
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_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.426
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.426
_diffrn_reflns_Laue_measured_fraction_max 0.966
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_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
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_diffrn_reflns_limit_l_min       -5
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_diffrn_reflns_point_group_measured_fraction_full 0.426
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         18.935
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_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.6304
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
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_exptl_crystal_description       needle
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_exptl_crystal_size_min          0.020
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         2956
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_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+2.0389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1430
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_reflns_number_total             2956
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           zhu211
_cod_original_cell_volume        3833(3)
_cod_original_sg_symbol_H-M      'P 21/c'
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_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.998
_shelxl_version_number           2014-3
_shelx_res_checksum              83909
_shelx_hkl_checksum              15491