Palladacycle catalysis: an innovation to the Suzuki-Miyaura cross-coupling reaction.
Lucio-Martínez, Fátima; Adrio, Luis A.; Polo-Ces, Paula; Ortigueira, Juan M.; Fernández, Jesús J; Adams, Harry; Pereira, M. Teresa; Vila, José M; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17598–17601; doi:10.1039/c6dt03542f

data_7040966
_publ_section_title
;
 Palladacycle catalysis: an innovation to the Suzuki-Miyaura
 cross-coupling reaction.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17598
_journal_page_last               17601
_journal_paper_doi               10.1039/c6dt03542f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H32 N3 O P Pd S'
_chemical_formula_sum            'C38 H36 N3 O2 P Pd S'
_chemical_formula_weight         736.13
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-10-02
_audit_creation_method
; 
Olex2 1.2-beta 
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) 
;
_audit_update_record
;
2016-10-13 deposited with the CCDC.
2016-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                107.932(2)
_cell_angle_beta                 95.926(2)
_cell_angle_gamma                104.175(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7093(13)
_cell_length_b                   11.0603(13)
_cell_length_c                   15.9546(19)
_cell_measurement_reflns_used    1300
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      3.5
_cell_measurement_theta_min      35.0
_cell_volume                     1710.2(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6711
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         1.999
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0350P)^2^+0.2690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4863
_reflns_number_total             6711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03542f2.cif
_cod_data_source_block           vi20la1n_sq_s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7040966.cif.
;
_cod_database_code               7040966
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.708
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Riding coordinates: 
 N3(H3) 
2.b Aromatic/amide H refined with riding coordinates: 
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C20(H20), C21(H21), 
 C22(H22), C23(H23), C024(H024), C25(H25), C26(H26), C27(H27), C28(H28), 
 C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C52(H52), C7C(H7C) 
2.c Idealised Me refined as rotating group: 
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C11(H10A,H10B,H10C) 
;
_shelx_fab_checksum              11484
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'