Synthesis, Structure, Dynamics, and Selective Methylation of Platinum and Palladium Diphosphametallacyclobutane Complexes
Chapp, Timothy W.; Schoenfeld, Adam J.; Sanderson, Matthew D.; Chang, Cory L.; Glueck, David S.; Golen, James A.; Moore, Curtis E.; Rheingold, Arnold L.; Organometallics 31 (2012) 5573–; doi:10.1021/om3005367

data_4078930
_publ_section_title
;
 Synthesis, Structure, Dynamics, and Selective Methylation of Platinum and
 Palladium Diphosphametallacyclobutane Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              5573
_journal_paper_doi               10.1021/om3005367
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C59 H78 P4 Pd, C4 H10 O, 2(C F3 O3 S)'
_chemical_formula_sum            'C65 H88 F6 O7 P4 Pd S2'
_chemical_formula_weight         1389.75
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
SHELXL-97

Notes 1) diethyl ether was disordered and refined as isotropic and O7 and C64
had large thermal amplitudes. Atom C60 and C61 were treated with EADP command
and the distances/angles of one the CF3SO3 anions were fixed with DIF/DANG.
While in no way was the quality of this structural determination compromised
by the level of completeness obtained, we have determined that its origin was
in the use of the then current version of the data collection strategy program
for high-symmetry data collections.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.4460(10)
_cell_length_b                   13.4460(10)
_cell_length_c                   66.635(7)
_cell_measurement_reflns_used    8685
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.03
_cell_measurement_theta_min      4.62
_cell_volume                     10433.2(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            49888
_diffrn_reflns_theta_full        66.13
_diffrn_reflns_theta_max         66.13
_diffrn_reflns_theta_min         4.63
_exptl_absorpt_coefficient_mu    4.122
_exptl_absorpt_correction_T_max  0.6376
_exptl_absorpt_correction_T_min  0.5081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4356
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.494
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         10176
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+3.8155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                9422
_reflns_number_total             10176
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005367_si_002.cif
_cod_data_source_block           glu338h
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        10433.2(15)
_cod_original_sg_symbol_Hall     'P 65 '
_cod_original_sg_symbol_H-M      P6(5)
_cod_database_code               4078930