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_4321387
_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            'C39 H37 Cl6 N O3 P2'
_chemical_formula_weight         842.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.86(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.183(3)
_cell_length_b                   11.645(4)
_cell_length_c                   16.791(6)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      8.71
_cell_measurement_theta_min      1.99
_cell_volume                     4003(2)
_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 .997
_diffrn_measured_fraction_theta_max .997
_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  0.0736
_diffrn_reflns_av_sigmaI/netI    0.1927
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10850
_diffrn_reflns_theta_full        22.52
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   'psi-scan corrections'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.092
_refine_diff_density_max         .442
_refine_diff_density_min         -.468
_refine_diff_density_rms         .047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         5225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0475
_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
 [0.00000+1.00000exp(7.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0500P)^2^+0.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1420
_reflns_number_gt                1900
_reflns_number_total             5225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000153n_1.cif
_cod_data_source_block           rtp997
_cod_database_code               4321387