The addition of bromine and iodine to palladacyclopentadienyl complexes bearing bidentate heteroditopic P-N spectator ligands derived from differently substituted quinolinic frames. The unexpected evolution of the reaction.
Canovese, Luciano; Visentin, Fabiano; Scattolin, Thomas; Santo, Claudio; Bertolasi, Valerio; Dalton transactions (Cambridge, England : 2003) 44 (2015) 15049–15058; doi:10.1039/c5dt01884f

data_7035872
_publ_section_title
;
 The addition of bromine and iodine to palladacyclopentadienyl complexes
 bearing bidentate heteroditopic P-N spectator ligands derived from
 differently substituted quinolinic frames. The unexpected evolution of
 the reaction.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15049
_journal_page_last               15058
_journal_paper_doi               10.1039/c5dt01884f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C34 H30 Br2 N O8 P Pd, C H2 Cl2'
_chemical_formula_sum            'C35 H32 Br2 Cl2 N O8 P Pd'
_chemical_formula_weight         962.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-12 deposited with the CCDC.
2015-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.5665(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7017(1)
_cell_length_b                   26.5544(3)
_cell_length_c                   12.1475(1)
_cell_measurement_reflns_used    40606
_cell_measurement_temperature    295
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.53
_cell_volume                     3710.61(6)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)''
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40606
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    2.892
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SORTAV (R.H.Blessing, Acta Cryst.,1995, A51, 33)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.145
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         10748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+3.6194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                8281
_reflns_number_total             10748
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c5dt01884f2.cif
_cod_data_source_block           DPPQ-Me-PdBr
_cod_depositor_comments
;Adding full bibliography for 7035871--7035873.cif.

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'contr' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        3710.60(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7035872