Chiral triazolylidene-Pd-PEPPSI: synthesis, characterization, and application in asymmetric Suzuki-Miyaura cross-coupling.
Haraguchi, Ryosuke; Hoshino, Shun; Yamazaki, Tatsuro; Fukuzawa, Shin-Ichi; Chemical communications (Cambridge, England) 54 (2018) 2110–2113; doi:10.1039/c7cc09960f

data_7121212
_publ_section_title
;
 Chiral triazolylidene-Pd-PEPPSI: synthesis, characterization, and
 application in asymmetric Suzuki-Miyaura cross-coupling.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2110
_journal_page_last               2113
_journal_paper_doi               10.1039/c7cc09960f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C34.67 H38.33 Cl4.33 Fe2 N4 Pd'
_chemical_formula_weight         882.74
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-21 deposited with the CCDC.
2018-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                120
_cell_formula_units_Z            9
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_cell_length_c                   16.877(2)
_cell_measurement_reflns_used    18831
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      31.4096
_cell_measurement_theta_min      2.6110
_cell_volume                     8160.5(18)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    'Yadokari-XG 2009(Wakita Nemoto et al.)'
_computing_publication_material  'Yadokari-XG 2009(Wakita,Nemoto et al.)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-2004
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0877
_diffrn_reflns_av_unetI/netI     0.1211
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
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_diffrn_reflns_number            60864
_diffrn_reflns_point_group_measured_fraction_full 0.995
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.129
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       Prism
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_exptl_crystal_size_mid          0.070
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_refine_diff_density_max         1.689
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 4298 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.055(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         21272
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0880
_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^)+(0.0689P)^2^+41.0741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2047
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                16792
_reflns_number_total             21272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09960f2.cif
_cod_data_source_block           ydkr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7121212.cif.
;
_cod_original_cell_volume        8160(2)
_cod_database_code               7121212
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.909
_shelx_res_checksum              41646