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_4085299
_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         'C48 H37 Br O P2 Pd'
_chemical_formula_sum            'C48 H37 Br O P2 Pd'
_chemical_formula_weight         878.02
_chemical_name_systematic
;
bromo((4-cyanophenyl)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'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 107.59(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.184(4)
_cell_length_b                   35.529(16)
_cell_length_c                   12.422(6)
_cell_measurement_reflns_used    9622
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7579
_cell_measurement_theta_min      2.8577
_cell_volume                     3864(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
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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
;
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 0.997
_diffrn_measured_fraction_theta_max 0.931
_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  0.0535
_diffrn_reflns_av_unetI/netI     0.0856
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27732
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.846
_diffrn_reflns_theta_min         2.867
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.634
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.771
_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            'light yellow'
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.2097
_exptl_crystal_size_mid          0.1617
_exptl_crystal_size_min          0.0608
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         9441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6142
_reflns_number_total             9441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501105w_si_001.cif
_cod_data_source_block           n292abs
_cod_depositor_comments
'Adding full bibliography for 4085296--4085300.cif.'
_cod_database_code               4085299
_shelxl_version_number           2013-4
_shelx_res_checksum              20851
_shelx_hkl_checksum              20838