Mono- and Dipalladated Derivatives of 2,5-Distyrylbenzene. Reactivity toward XyNC and Alkynes. Synthesis of Complexes with Indacenediide Ligands
Fernández-Rodr\?íguez, Mar\?ía-José; Mart\?ínez-Viviente, Elo\?ísa; Vicente, José; Jones, Peter G.; Organometallics 34 (2015) 2240–; doi:10.1021/om5010034

data_4084839
_publ_section_title
;
 Mono- and Dipalladated Derivatives of 2,5-Distyrylbenzene. Reactivity
 toward XyNC and Alkynes. Synthesis of Complexes with Indacenediide
 Ligands
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2240
_journal_paper_doi               10.1021/om5010034
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C95 H84 Cl21 D7 F6 N4 O6 Pd2 S2'
_chemical_formula_weight         2527.13
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.271(4)
_cell_angle_beta                 74.026(4)
_cell_angle_gamma                88.309(4)
_cell_formula_units_Z            2
_cell_length_a                   14.4062(12)
_cell_length_b                   19.8994(16)
_cell_length_c                   22.0291(18)
_cell_measurement_reflns_used    9193
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.75
_cell_measurement_theta_min      2.34
_cell_volume                     5439.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.1036
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76772
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.9542
_exptl_absorpt_correction_T_min  0.7892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dichroic, blue-green/orange'
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.666
_refine_diff_density_min         -2.824
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         24845
_refine_ls_number_restraints     1823
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+24.9198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.2010
_reflns_number_gt                15574
_reflns_number_total             24845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5010034_si_002.cif
_cod_data_source_block           vite
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (74
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26 (170
times).

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4084839--4084842.cif.
;
_cod_original_formula_sum        'C95 H84 D7 Cl21 F6 N4 O6 Pd2 S2'
_cod_database_code               4084839