α-Diimine synthesis via titanium-mediated multicomponent diimination of alkynes with C-nitrosos
Frye, Connor W.; Egger, Dominic T.; Kounalis, Errikos; Pearce, Adam J.; Cheng, Yukun; Tonks, Ian A.; Chemical Science 13 (2022) 1469–1477; doi:10.1039/D1SC06111A

data_1565840
_publ_section_title
;
 \a-Diimine synthesis via titanium-mediated multicomponent diimination of
 alkynes with C-nitrosos
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              1469
_journal_page_last               1477
_journal_paper_doi               10.1039/D1SC06111A
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C21H18Cl2N2Zn CHCl3'
_chemical_formula_sum            'C22 H19 Cl5 N2 Zn'
_chemical_formula_weight         554.01
_chemical_name_common            21011
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-03-22 deposited with the CCDC.	2021-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_volume                     4818.4(7)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX3, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'Shelxle-(Rev. 825) (Huebschle, C. B., 2011)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Photon-II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1048
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61367
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.944
_diffrn_reflns_theta_min         2.034
_diffrn_source                   micro
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CDCl3'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6228
_refine_diff_density_max         1.609
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         11497
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1155P)^2^+0.3830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7010
_reflns_number_total             11497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06111a2.cif
_cod_data_source_block           21011_corr
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1565840.cif.
;
_cod_original_cell_volume        4818.4(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565840
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.857
_shelx_estimated_absorpt_t_max   0.857
_shelx_res_checksum              4801
_shelx_hkl_checksum              80436