Palladium End-Capped Polyynes via Oxidative Addition of 1-Haloalkynes to Pd(PPh3)4
Gulia, Nurbey; Pigulski, Bartłomiej; Szafert, Sławomir; Organometallics 34 (2015) 673–; doi:10.1021/om501105w

data_4085297
_publ_section_title
;
 Palladium End-Capped Polyynes via Oxidative Addition of 1-Haloalkynes to
 Pd(PPh3)4
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              673
_journal_paper_doi               10.1021/om501105w
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C44 H34 Br N O2 P2 Pd'
_chemical_formula_sum            'C44 H34 Br N O2 P2 Pd'
_chemical_formula_weight         856.97
_chemical_name_systematic
;
bromo((4-nitrophenyl)ethynyl)bis(triphenylphosphine)palladium
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.05(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.032(5)
_cell_length_b                   19.823(9)
_cell_length_c                   19.438(9)
_cell_measurement_reflns_used    14467
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9998
_cell_measurement_theta_min      2.8761
_cell_volume                     3806(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.1449
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54021
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.062
_diffrn_reflns_theta_min         2.882
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.4803
_exptl_crystal_size_mid          0.1399
_exptl_crystal_size_min          0.0200
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 4162 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.333(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.810
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         19977
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.810
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    0.848
_reflns_Friedel_fraction_max     0.798
_reflns_number_gt                12720
_reflns_number_total             19977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501105w_si_001.cif
_cod_data_source_block           ngu1abs2
_cod_depositor_comments
'Adding full bibliography for 4085296--4085300.cif.'
_cod_database_code               4085297
_shelxl_version_number           2013-4
_shelx_res_checksum              40573
_shelx_hkl_checksum              91722