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_4079386
_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            'C26 H38 P2 Pt'
_chemical_formula_weight         607.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_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                70.5860(10)
_cell_angle_beta                 71.854(2)
_cell_angle_gamma                86.595(2)
_cell_formula_units_Z            4
_cell_length_a                   10.4386(4)
_cell_length_b                   15.8857(7)
_cell_length_c                   16.7485(8)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.71
_cell_volume                     2486.11(19)
_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 0.971
_diffrn_measured_fraction_theta_max 0.959
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51834
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    5.783
_exptl_absorpt_correction_T_max  0.5687
_exptl_absorpt_correction_T_min  0.3374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.010
_refine_diff_density_min         -1.707
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1046
_refine_ls_number_reflns         18734
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                16709
_reflns_number_total             18734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300704e_si_002.cif
_cod_data_source_block           glu378
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      P1
_cod_database_code               4079386
_alert_comments
;
The A-level alert for this structure arises from atoms with unusual thermal ellipsoids.
Instead of adding restraints, we prefer to report these results directly as 
they appear from the data.
;