C(alkenyl)-H Activation via Six-Membered Palladacycles: Catalytic 1,3-Diene Synthesis.
Liu, Mingyu; Yang, Pusu; Karunananda, Malkanthi K.; Wang, Yanyan; Liu, Peng; Engle, Keary M.; Journal of the American Chemical Society 140 (2018) 5805–5813; doi:10.1021/jacs.8b02124

data_4132172
_publ_section_title
;
 C(alkenyl)-H Activation via Six-Membered Palladacycles: Catalytic
 1,3-Diene Synthesis.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5805
_journal_page_last               5813
_journal_paper_doi               10.1021/jacs.8b02124
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C26 H22 N2 O3 Pd, 0.5(C2 H4 Cl2)'
_chemical_formula_sum            'C27 H24 Cl N2 O3 Pd'
_chemical_formula_weight         566.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-11-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                110.579(2)
_cell_angle_beta                 96.643(2)
_cell_angle_gamma                90.227(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0696(6)
_cell_length_b                   10.1472(7)
_cell_length_c                   11.9906(7)
_cell_measurement_reflns_used    5181
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.344
_cell_measurement_theta_min      2.889
_cell_volume                     1137.98(12)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17028
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_min         1.828
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.2293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0532 before and 0.0462 after correction. The Ratio of minimum to maximum transmission is 0.8812. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       Block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0232P)^2^+0.7297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3986
_reflns_number_total             4638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02124_si_003.cif
_cod_data_source_block           Engle64
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_exptl_crystal_colour_primary' value 'Yellow' was changed
to 'yellow' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/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_database_code               4132172
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1S) = Uanis(C1SB)
3. Others
 Sof(C1SB)=Sof(H1SC)=Sof(H1SD)=1-FVAR(1)
 Sof(C1S)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C1S(H1SA,H1SB), C1SB(H1SC,H1SD)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C8(H8), C9(H9), C10(H10), C15(H15), C26(H26), C19(H19),
 C22(H22), C18(H18), C23(H23), C24(H24), C25(H25)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              91329
_shelx_hkl_checksum              36053
_olex2_submission_special_instructions 'No special instructions were received'