Synthesis, Characterization, and Coordination Chemistry of a New Geometrically Hindered Trifunctional Ligand, 4,5-Bis(diphenylphosphino)-sym-octahydroacridine N,P,P'-Trioxide
Gan, Xin-Min; Parveen, Sahrah; Smith, Wayne L.; Duesler, Eileen N.; Paine, Robert T.; Inorganic Chemistry 39 (2000) 4591–4598; doi:10.1021/ic000153n

data_4321390
_publ_contact_author             'Robert T. Paine'
_publ_contact_author_email       rtpaine@unm.edu
_publ_contact_author_fax         1.505.277.2609
_publ_contact_author_phone       1.505.277.1661
_publ_section_title
;
 Synthesis, Characterization, and Coordination Chemistry of a New
 Geometrically Hindered Trifunctional Ligand,
 4,5-Bis(diphenylphosphino)-sym-octahydroacridine N,P,P'-Trioxide
;
_journal_coden_ASTM              JACSAT
_journal_issue                   20
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4591
_journal_page_last               4598
_journal_paper_doi               10.1021/ic000153n
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C38 H39 N4 Nd O13 P2'
_chemical_formula_weight         965.91
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.131(2)
_cell_length_b                   17.579(8)
_cell_length_c                   17.853(7)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10.98
_cell_measurement_theta_min      2.28
_cell_volume                     4121(3)
_computing_cell_refinement       'XSCANS V2.2 (Siemens, 1994)'
_computing_data_collection       'XSCANS V2.2 (Siemens, 1994)'
_computing_data_reduction        'XSCANS V2.2 (Siemens, 1994)'
_computing_molecular_graphics    'SHELXTL V5.0 (Siemens, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'profile data from \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  0.0797
_diffrn_reflns_av_sigmaI/netI    0.2064
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -12
_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            8105
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.406
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_correction_T_min  0.9406
_exptl_absorpt_correction_type   'Gaussian Face-Indexed'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.046
_refine_diff_density_max         .367
_refine_diff_density_min         -.462
_refine_diff_density_rms         .068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         3845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [0.00000+1.00000exp(9.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0200P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                2037
_reflns_number_total             3845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000153n_4.cif
_cod_data_source_block           rtp999a
_cod_database_code               4321390