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_4078928
_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_formula_sum            'C57 H72 P4 Pt'
_chemical_formula_weight         1076.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 121.312(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.135(4)
_cell_length_b                   9.8628(10)
_cell_length_c                   18.4542(19)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.34
_cell_volume                     5152.5(10)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX 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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4737
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    2.883
_exptl_absorpt_correction_T_max  0.6716
_exptl_absorpt_correction_T_min  0.4234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.635
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+32.0657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                4342
_reflns_number_total             4737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005367_si_002.cif
_cod_data_source_block           glu306_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        5152.5(9)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4078928