A hybrid silylene-Pd catalyst: efficient C-N cross-coupling of sterically bulky amines and chiral amines.
Kaulage, Sandeep H.; Parvin, Nasrina; Khopade, Kishor V.; Khan, Shabana; Chemical communications (Cambridge, England) 60 (2024) 9958–9961; doi:10.1039/d4cc03108c

data_7133523
_publ_section_title
;
 A hybrid silylene-Pd catalyst: efficient C-N cross-coupling of sterically
 bulky amines and chiral amines.
;
_journal_issue                   73
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9958
_journal_page_last               9961
_journal_paper_doi               10.1039/d4cc03108c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C36 H46 Cl2 N3 P Pd Si2, C H2 Cl2'
_chemical_formula_sum            'C37 H48 Cl4 N3 P Pd Si2'
_chemical_formula_weight         870.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_audit_update_record
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2024-08-08 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2289
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_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
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_diffrn_reflns_number            125014
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.101
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_diffrn_reflns_theta_min         2.553
_diffrn_source_current           1.0
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2016'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.294
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_refine_ls_R_factor_gt           0.0738
_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^)+104.7596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4647
_reflns_number_total             7861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03108c2.cif
_cod_data_source_block           3
_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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133516--7133523.cif.
;
_cod_database_code               7133523
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C73(H73A,H73B)
1.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32)
1.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31643
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_shelx_fab_checksum              38639
_olex2_submission_special_instructions 'No special instructions were received'