Synthesis of unsymmetrical NCN′ and PCN pincer palladacycles and their catalytic evaluation compared with a related SCN pincer palladacycle
Roffe, Gavin W.; Tizzard, Graham J.; Coles, Simon J.; Cox, Hazel; Spencer, John; Organic Chemistry Frontiers 3 (2016) 957–; doi:10.1039/C6QO00198J

data_1553470
_publ_section_title
;
 Synthesis of unsymmetrical NCN&#x2032; and PCN pincer palladacycles and
 their catalytic evaluation compared with a related SCN pincer
 palladacycle
;
_journal_issue                   8
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              957
_journal_paper_doi               10.1039/C6QO00198J
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C16 H17 Cl N2 O Pd'
_chemical_formula_sum            'C16 H17 Cl N2 O Pd'
_chemical_formula_weight         395.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
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2014-12-10 deposited with the CCDC.
2016-06-08 downloaded from the CCDC.
;
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_cell_volume                     1446.33(18)
_computing_cell_refinement
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
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'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
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_computing_structure_solution
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
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_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
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_diffrn_measured_fraction_theta_full 0.998
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_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
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_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_theta_max         27.484
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_diffrn_source                   'Rotating Anode'
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_diffrn_source_target            Mo
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_diffrn_source_voltage           45.0
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CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_exptl_crystal_colour            Colourless
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_refine_ls_R_factor_all          0.0249
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+2.4212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                3077
_reflns_number_total             3305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qo00198j2.cif
_cod_data_source_block           4c
_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/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/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 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C16 H17 Cl1 N2 O1 Pd1 '
_cod_database_code               1553470
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9)
;
_shelx_res_checksum              5902
_shelx_hkl_checksum              47549