Structure and Thermal Reactivity of a Novel Pd(0) Metalloenediyne
Nicole L. Coalter; Thomas E. Concolino; William E. Streib; Chris G. Hughes; Arnold L. Rheingold; Jeffrey M. Zaleski; Journal of the American Chemical Society 122 (2000) 3112–3117; doi:10.1021/ja9944094

data_4115970
_publ_contact_author
;
     Dr. Jeffrey M. Zaleski
     Department of Chemistry
     Indiana University
     Bloomington, IN 47405
     USA
;
_publ_contact_author_email       zaleski@indiana.edu
_publ_contact_author_fax         '+812 855 7148'
_publ_contact_author_phone       '+812 855 2134'
_publ_section_title
;
 Structure and Thermal Reactivity of a Novel Pd(0) Metalloenediyne
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3112
_journal_page_last               3117
_journal_paper_doi               10.1021/ja9944094
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C68 H48 Cl N O3 P4 Pd2'
_chemical_formula_weight         1299.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.1406(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4456(2)
_cell_length_b                   18.5241(2)
_cell_length_c                   14.3865(2)
_cell_measurement_temperature    173(2)
_cell_volume                     2970.35(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9461
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.8555
_exptl_absorpt_correction_T_min  0.7941
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.594
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.237
_refine_ls_extinction_coef       0.081(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   3.540
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         3866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      3.540
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.1277
_refine_ls_shift/su_max          0.096
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4027
_refine_ls_wR_factor_ref         0.4067
_reflns_number_gt                3578
_reflns_number_total             3866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9944094.cif
_cod_data_source_block           zal03
_cod_original_cell_volume        2970.35(4)
_cod_database_code               4115970