Novel chiral 1,5-diaza-3,7-diphosphacyclooctane ligands and their transition metal complexes
Andrey A. Karasik; Roman N. Naumov; Oleg G. Sinyashin; Gennadii P. Belov; Helena V. Novikova; Peter Lönnecke; Evamarie Hey-Hawkins; Dalton Trans.  (2003) 2209–2214; doi:10.1039/b300754e

data_7012742
_publ_section_title
;
 Novel chiral 1,5-diaza-3,7-diphosphacyclooctane ligands and their
 transition metal complexes
;
_journal_issue                   11
_journal_name_full               'Dalton Trans.'
_journal_page_first              2209
_journal_page_last               2214
_journal_paper_doi               10.1039/b300754e
_journal_year                    2003
_chemical_formula_sum            'C32 H36 N2 P2'
_chemical_formula_weight         510.57
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 100.552(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.052(12)
_cell_length_b                   5.472(3)
_cell_length_c                   22.567(12)
_cell_measurement_reflns_used    1200
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.089
_cell_measurement_theta_min      2.326
_cell_volume                     2798(3)
_computing_cell_refinement       'SAINT (AXS Bruker)'
_computing_data_collection       'SMART (AXS Bruker)'
_computing_data_reduction        'SAINT (AXS Bruker)'
_computing_molecular_graphics    'XP (AXS Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHESXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD-Diffractometer (AXS Bruker)'
_diffrn_measurement_method       'Omega 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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.1257
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8210
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_correction_T_min  0.9652
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5349
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.0718
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+3.3458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                3256
_reflns_number_total             5349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300754e.txt
_cod_data_source_block           c988_fin
_cod_original_cell_volume        2799(2)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               7012742