New cycloimmonium ylide ligands and their palladium(ii) affinities
Postolachi, Rodica; Danac, Ramona; Buurma, Niklaas J.; Pui, Aurel; Balan, Mihaela; Shova, Sergiu; Deleanu, Calin; RSC Advances 3 (2013) 17260–; doi:10.1039/c3ra41911h

data_7239084
_publ_section_title
;
 New cycloimmonium ylide ligands and their palladium(ii) affinities
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              17260
_journal_paper_doi               10.1039/c3ra41911h
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C26 H20 Br N3 O2 S'
_chemical_formula_sum            'C26 H20 Br N3 O2 S'
_chemical_formula_weight         518.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-19
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled Nov  7 2012 10:32:32, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.698(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.705(2)
_cell_length_b                   21.458(2)
_cell_length_c                   12.8736(9)
_cell_measurement_reflns_used    922
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4346
_cell_measurement_theta_min      2.8684
_cell_volume                     4548.7(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -41.00   53.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.3503   77.0000  -30.0000 94

  2 omega  -10.00   83.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       17.0065   77.0000 -150.0000 93
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0308738000
_diffrn_orient_matrix_UB_12      0.0189857000
_diffrn_orient_matrix_UB_13      -0.0150349000
_diffrn_orient_matrix_UB_21      0.0300797000
_diffrn_orient_matrix_UB_22      -0.0193922000
_diffrn_orient_matrix_UB_23      0.0292744000
_diffrn_orient_matrix_UB_31      0.0002336000
_diffrn_orient_matrix_UB_32      -0.0188592000
_diffrn_orient_matrix_UB_33      -0.0451508000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1509
_diffrn_reflns_av_unetI/netI     0.3352
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17784
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.929
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.3011
_refine_ls_R_factor_gt           0.0868
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                2735
_reflns_number_total             8866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41911h.txt
_cod_data_source_block           shi_319_aupu
_cod_original_cell_volume        4548.6(8)
_cod_database_code               7239084
_chemical_oxdiff_formula         'C52 H30 Mn1 N2 Cl4 O2'
_chemical_oxdiff_usercomment     Mn_R5
_reflns_odcompleteness_completeness 98.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H24B of C24B, H15A of C15A, H6B of C6B, H18A of C18A, H2A of C2A, H12B of
  C12B, H25A of C25A, H15B of C15B, H26B of C26B, H26A of C26A, H11A of C11A,
  H21B of C21B, H3A of C3A, H11B of C11B, H16A of C16A, H20B of C20B, H23B of
  C23B, H16B of C16B, H25B of C25B, H6A of C6A, H17A of C17A, H17B of C17B, H3B
  of C3B, H2B of C2B, H5A of C5A, H23A of C23A, H18B of C18B, H1A of N1A, H1B
  of N1B, H20A of C20A, H21A of C21A, H5B of C5B, H24A of C24A, H12A of C12A
 At 1.5 times of:
  {H14A,H14B,H14C} of C14B, {H14D,H14E,H14F} of C14A
2.a Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N1B(H1B), C20A(H20A), C21A(H21A), C17B(H17B), C3B(H3B), C2B(H2B),
 C5A(H5A), C23A(H23A), C18B(H18B), C15A(H15A), C25B(H25B), C17A(H17A),
 C18A(H18A), C12A(H12A), C6A(H6A), C20B(H20B), C16A(H16A), C24A(H24A),
 C23B(H23B), C16B(H16B), C5B(H5B), C24B(H24B), C6B(H6B), C2A(H2A), C12B(H12B),
 C25A(H25A), C26A(H26A), C11B(H11B), C15B(H15B), C11A(H11A), C26B(H26B),
 C21B(H21B), C3A(H3A)
2.b Idealised Me refined as rotating group:
 C14B(H14A,H14B,H14C), C14A(H14D,H14E,H14F)
;