Synthesis and Coordination Chemistry of a Tridentateo-Phenylene-Bridged Diphosphine−NHC System
Steinke, Tobias; Shaw, Bryan K.; Jong, Howard; Patrick, Brian O.; Fryzuk, Michael D.; Organometallics 28 (2009) 2830–; doi:10.1021/om9000764

data_4069221
_publ_section_title
;
 Synthesis and Coordination Chemistry of a Tridentateo-Phenylene-Bridged
 Diphosphine&#x2212;NHC System
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2830
_journal_paper_doi               10.1021/om9000764
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C31 H49 F6 N2 O P3 Pd'
_chemical_formula_sum            'C31 H49 F6 N2 O P3 Pd'
_chemical_formula_weight         779.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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                83.175(4)
_cell_angle_beta                 79.282(4)
_cell_angle_gamma                78.507(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4942(10)
_cell_length_b                   14.7569(19)
_cell_length_c                   15.813(2)
_cell_measurement_reflns_used    6010
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.031
_cell_measurement_theta_min      2.4745
_cell_volume                     1901.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker X8 Apex 2'
_diffrn_measurement_method       'area detector'
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17216
_diffrn_reflns_theta_full        23.69
_diffrn_reflns_theta_max         23.69
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.9353
_exptl_absorpt_correction_T_min  0.8078
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.685
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5203
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+18.3271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1848
_reflns_number_gt                4293
_reflns_number_total             5203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9000764_si_004.cif
_cod_data_source_block           mf674
_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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069221