Syntheses of Tetrahydropyridazine and Tetrahydro-1,2-diazepine Scaffolds through Cycloaddition Reactions of Azoalkenes with Enol Diazoacetates.
Deng, Yongming; Pei, Chao; Arman, Hadi; Dong, Kuiyong; Xu, Xinfang; Doyle, Michael P.; Organic letters 18 (2016) 5884–5887; doi:10.1021/acs.orglett.6b02965

data_1544523
_publ_section_title
;
 Syntheses of Tetrahydropyridazine and Tetrahydro-1,2-diazepine Scaffolds
 through Cycloaddition Reactions of Azoalkenes with Enol Diazoacetates.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              5884
_journal_page_last               5887
_journal_paper_doi               10.1021/acs.orglett.6b02965
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C26 H32 N4 O4 Si'
_chemical_formula_sum            'C26 H32 N4 O4 Si'
_chemical_formula_weight         492.64
_chemical_name_systematic
;
 ?
;
_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'
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_cell_measurement_reflns_used    9023
_cell_measurement_temperature    273(2)
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_cell_measurement_theta_min      2.32
_cell_volume                     2704.0(10)
_computing_cell_refinement       'Bruker SAINT'
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_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      273(2)
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_diffrn_measured_fraction_theta_max 0.994
_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_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            125079
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_diffrn_reflns_point_group_measured_fraction_max 0.994
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_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         2.432
_diffrn_source                   'microfocus sealed tube'
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
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_exptl_transmission_factor_min   0.985
_refine_diff_density_max         1.640
_refine_diff_density_min         -0.678
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         12413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1193P)^2^+1.8657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2095
_refine_ls_wR_factor_ref         0.2355
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8538
_reflns_number_total             12413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b02965_si_004.cif
_cod_data_source_block           dk41_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1544521--1544523.cif.

 Adding full bibliography for 1544521--1544523.cif.
;
_cod_original_cell_volume        2704.2(10)
_cod_database_code               1544523
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2014-3
_shelx_res_checksum              53492
_shelx_hkl_checksum              93068