Synthesis and Structure of Platinum Bis(phospholane) Complexes Pt(diphos*)(R)(X), Catalyst Precursors for Asymmetric Phosphine Alkylation
Guino-o, Marites A.; Zureick, Andrew H.; Blank, Natalia F.; Anderson, Brian J.; Chapp, Timothy W.; Kim, Youngmin; Glueck, David S.; Rheingold, Arnold L.; Organometallics 31 (2012) 6900–; doi:10.1021/om300704e

data_4079384
_publ_section_title
;
 Synthesis and Structure of Platinum Bis(phospholane) Complexes
 Pt(diphos*)(R)(X), Catalyst Precursors for Asymmetric Phosphine
 Alkylation
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6900
_journal_paper_doi               10.1021/om300704e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C14 H28 Cl2 O0 P2 Pt'
_chemical_formula_weight         524.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 97.173(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2371(12)
_cell_length_b                   12.4943(19)
_cell_length_c                   10.0870(15)
_cell_measurement_reflns_used    1478
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.94
_cell_measurement_theta_min      15.78
_cell_volume                     905.0(2)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.849
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1196
_diffrn_reflns_av_sigmaI/netI    0.1325
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5098
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         70.27
_diffrn_reflns_theta_min         15.78
_exptl_absorpt_coefficient_mu    18.767
_exptl_absorpt_correction_T_max  0.692
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.881
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.289
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2491
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+2.8218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1693
_reflns_number_gt                2280
_reflns_number_total             2491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300704e_si_002.cif
_cod_data_source_block           glu360
_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_sg_symbol_H-M      P2(1)
_cod_database_code               4079384
_alert_comments_
; 
The A-level alert arises from the overall weakness of data and our inability
to obtain an acceptable (by CHECKCIF standards) amount of high-angle data.  
Nonetheless, we are confident this remains a fully acceptable structure.
;