Synthesis and Coordination Chemistry of the First C2-Chiral Bisoxazine Ligand
Clément Mazet; Lutz H. Gade; Inorganic Chemistry 42 (2003) 210–215; doi:10.1021/ic025947b

data_4312898
_publ_section_title
;
 Synthesis and Coordination Chemistry of the First C2-Chiral Bisoxazine
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              210
_journal_page_last               215
_journal_paper_doi               10.1021/ic025947b
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety
'C36 H52 Cl2 N6 O4 Pd2,C36 H52 Cl2 N6 O4 Pd2 '
_chemical_formula_sum            'C72 H104 Cl4 N12 O8 Pd4'
_chemical_formula_weight         1833.12
_chemical_name_systematic        ' ?'
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_date             17-06-02
_cell_angle_alpha                78.859(5)
_cell_angle_beta                 72.529(5)
_cell_angle_gamma                72.664(5)
_cell_formula_units_Z            1
_cell_length_a                   9.8399(3)
_cell_length_b                   13.7785(6)
_cell_length_c                   15.9563(7)
_cell_measurement_reflns_used    11386
_cell_measurement_temperature    294
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     1956.97(15)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      294
_diffrn_measurement_details
;
   2100 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  1.0 deg 1 scans of   60 sec per frame.
 Data collection was divided into  1 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00  123 frames
 Friedel pairs were averaged. Internal R = 0.02
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11386
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7111
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.56
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.113
_refine_diff_density_min         -0.174
_refine_ls_abs_structure_details 'Flack H D  (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   11.127
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     886
_refine_ls_number_reflns         7215
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.080
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/esd_mean        0.010
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.482
_refine_ls_wR_factor_ref         0.056
_reflns_number_gt                7215
_reflns_number_total             11386
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ic025947b_s1.cif
_cod_data_source_block           st893B
_cod_original_cell_volume        1957.0(1)
_cod_database_code               4312898