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_4319291
_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            'C46 H55 As O3'
_chemical_formula_weight         730.82
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   26.4932(14)
_cell_length_b                   26.4932(14)
_cell_length_c                   27.759(2)
_cell_measurement_temperature    173(2)
_cell_volume                     16873.4(18)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1123
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            38882
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.874862
_exptl_absorpt_correction_T_min  0.641992
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             6984
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         9227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                7176
_reflns_number_total             9227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000683j_2.cif
_cod_data_source_block           3b
_cod_original_cell_volume        16873.6(18)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4319291