Capturing a Ghost. Synthesis and Structural Characterization of Pd(dba)[P(o-Tol)3]2
Harding, Brennen A.; Melvin, Patrick R.; Dougherty, William; Kassel, Scott; Goodson, Felix E.; Organometallics 32 (2013) 3570–; doi:10.1021/om400335a

data_4089519
_publ_section_title
;
 Capturing a Ghost. Synthesis and Structural Characterization of
 Pd(dba)[P(o-Tol)3]2
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3570
_journal_paper_doi               10.1021/om400335a
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C65 H71 O2.5 P2 Pd'
_chemical_formula_weight         1060.56
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.671(3)
_cell_angle_beta                 84.162(3)
_cell_angle_gamma                83.843(3)
_cell_formula_units_Z            2
_cell_length_a                   13.744(2)
_cell_length_b                   13.865(2)
_cell_length_c                   14.555(2)
_cell_measurement_reflns_used    8259
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      32.95
_cell_measurement_theta_min      2.58
_cell_volume                     2737.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            80432
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.9655
_exptl_absorpt_correction_T_min  0.9168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             1114
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         20641
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.6360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                15004
_reflns_number_total             20641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400335a_si_002.cif
_cod_data_source_block           good004
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2737.6(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C65 H71 O2.50 P2 Pd'
_cod_database_code               4089519