Hydrothermal in situ ligand reaction: copper(II)-mediated stepwise oxidation of 2,3,5- and 2,4,6-trimethylpyridine to pyridinecarboxylates
Li, Cui-Jin; Lin, Zhuojia; Yun, Lei; Xie, Yu-Ling; Leng, Ji-Dong; Ou, Yong-Cong; Tong, Ming-Liang; CrystEngComm 12 (2010) 425–; doi:10.1039/b911463g

data_7211638
_publ_section_title
;
 Hydrothermal in situ ligand reaction: copper(II)-mediated stepwise
 oxidation of 2,3,5- and 2,4,6-trimethylpyridine to pyridinecarboxylates
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              425
_journal_paper_doi               10.1039/b911463g
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C8 H8 N2 O8'
_chemical_formula_weight         260.16
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.703(11)
_cell_angle_beta                 80.971(10)
_cell_angle_gamma                80.399(9)
_cell_formula_units_Z            2
_cell_length_a                   4.8656(5)
_cell_length_b                   9.7640(12)
_cell_length_c                   11.1677(14)
_cell_measurement_reflns_used    672
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      61.5450
_cell_measurement_theta_min      4.1467
_cell_volume                     498.69(11)
_computing_cell_refinement
;
'Wed Jun 27 14:31:55 2007'
;
_computing_data_collection
;
'Wed Jun 27 14:31:55 2007'
;
_computing_data_reduction
;
'Wed Jun 27 14:31:55 2007'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 16.0855
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Gemini S Ultra'
_diffrn_measurement_method       '\w and \p scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2420
_diffrn_reflns_theta_full        61.43
_diffrn_reflns_theta_max         61.43
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  0.8169
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'Wed Jun 27 14:31:55 2007'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         1401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0880
_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^)+(0.1255P)^2^+2.1333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2504
_refine_ls_wR_factor_ref         0.2658
_reflns_number_gt                972
_reflns_number_total             1401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b911463g.txt
_cod_data_source_block           ligand
_cod_original_cell_volume        498.69(10)
_cod_database_code               7211638