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_4085298
_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         'C46 H34 Br N O2 P2 Pd'
_chemical_formula_sum            'C46 H34 Br N O2 P2 Pd'
_chemical_formula_weight         880.99
_chemical_name_systematic
;
bromo((4-nitrophenyl)butadiynyl)bis(triphenylphosphine)palladium
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
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_cell_angle_alpha                90
_cell_angle_beta                 108.02(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.281(3)
_cell_length_b                   35.018(12)
_cell_length_c                   12.200(4)
_cell_measurement_reflns_used    6462
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.4986
_cell_measurement_theta_min      2.5812
_cell_volume                     3771(2)
_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
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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
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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 8.1956
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_unetI/netI     0.1950
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32808
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.772
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_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            'light yellow'
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.1885
_exptl_crystal_size_mid          0.1542
_exptl_crystal_size_min          0.0150
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         10599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5038
_reflns_number_total             10599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501105w_si_001.cif
_cod_data_source_block           n233abs
_cod_depositor_comments
'Adding full bibliography for 4085296--4085300.cif.'
_cod_database_code               4085298
_shelxl_version_number           2013-4
_shelx_res_checksum              74902
_shelx_hkl_checksum              87293