Sterically Crowded, Rigid,C3 Symmetric Phosphites: Synthesis, Structure, and Preparation of Metal Complexes
Maarten B. Dinger; Michael J. Scott; Inorganic Chemistry 40 (2001) 856–864; doi:10.1021/ic000683j

data_4319292
_publ_contact_author_address
;
P.O. Box 117200
University of Florida
Gainesville FL, 32611
;
_publ_contact_author_name        'Maarten B. Dinger and Michael J. Scott'
_publ_section_title
;
 Sterically Crowded, Rigid,C3 Symmetric Phosphites: Synthesis, Structure,
 and Preparation of Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              856
_journal_page_last               864
_journal_paper_doi               10.1021/ic000683j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C93.75 H129.75 Cl27.25 O6 P2 Pd2'
_chemical_formula_weight         2593.48
_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                70.109(2)
_cell_angle_beta                 74.658(2)
_cell_angle_gamma                81.012(2)
_cell_formula_units_Z            4
_cell_length_a                   18.2064(16)
_cell_length_b                   25.301(2)
_cell_length_c                   29.814(3)
_cell_measurement_temperature    173(2)
_cell_volume                     12420.8(19)
_computing_cell_refinement       'Bruker AXS SMART'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.1119
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54849
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         0.75
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.672552
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin shard'
_exptl_crystal_F_000             5302
_refine_diff_density_max         1.514
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.00022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2138
_refine_ls_number_reflns         32397
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2312
_refine_ls_wR_factor_ref         0.2623
_reflns_number_gt                19993
_reflns_number_total             32397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000683j_3.cif
_cod_data_source_block           4a
_cod_original_cell_volume        12420.6(19)
_cod_database_code               4319292