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_4319293
_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            'C37 H48 Cl O3 P Pd'
_chemical_formula_weight         713.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.9800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.4765(11)
_cell_length_b                   21.4850(14)
_cell_length_c                   18.7477(11)
_cell_measurement_temperature    173(2)
_cell_volume                     6971.3(8)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47538
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.951583
_exptl_absorpt_correction_T_min  0.818756
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             2976
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         15995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                9566
_reflns_number_total             15995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000683j_4.cif
_cod_data_source_block           5b
_cod_database_code               4319293