Palladacycle containing nitrogen and selenium: highly active pre-catalyst for the Suzuki-Miyaura coupling reaction and unprecedented conversion into nano-sized Pd17Se15.
Rao, Gyandshwar Kumar; Kumar, Arun; Ahmed, Jahangeer; Singh, Ajai Kumar; Chemical communications (Cambridge, England) 46 (2010) 5954–5956; doi:10.1039/c0cc01075h

data_7113077
_publ_section_title
;
 Palladacycle containing nitrogen and selenium: highly active pre-catalyst
 for the Suzuki-Miyaura coupling reaction and unprecedented conversion
 into nano-sized Pd17Se15.
;
_journal_issue                   32
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5954
_journal_page_last               5956
_journal_paper_doi               10.1039/c0cc01075h
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C22 H22 Cl N O Pd Se, B H3 O3'
_chemical_formula_sum            'C22 H25 B Cl N O4 Pd Se'
_chemical_formula_weight         599.05
_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                67.335(9)
_cell_angle_beta                 86.782(9)
_cell_angle_gamma                70.283(9)
_cell_formula_units_Z            2
_cell_length_a                   8.713(5)
_cell_length_b                   12.599(7)
_cell_length_c                   12.850(7)
_cell_measurement_reflns_used    2769
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.57
_cell_measurement_theta_min      2.49
_cell_volume                     1220.9(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  '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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11512
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    2.377
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_meas      1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rods
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.463
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                3420
_reflns_number_total             4248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01075h.txt
_cod_data_source_block           gyan3m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1221.0(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7113077