Temperature-Dependent in Situ Reduction of 4,4′-Azobispyridine via Solvothermal Reaction
Gai, Yan-Li; Jiang, Fei-Long; Xiong, Ke-Cai; Chen, Lian; Yuan, Da-Qiang; Zhang, Lin-Jie; Zhou, Kang; Hong, Mao-Chun; Crystal Growth & Design 12 (2012) 2079–; doi:10.1021/cg3000813

data_4506015
_publ_section_title
;
 Temperature-Dependent in Situ Reduction of 4,4&#x2032;-Azobispyridine via
 Solvothermal Reaction
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2079
_journal_paper_doi               10.1021/cg3000813
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C24 H19 Mn N4 O5.5'
_chemical_formula_weight         506.37
_chemical_name_systematic
; 
 ? 
;
_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                 110.910(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.185(7)
_cell_length_b                   13.588(5)
_cell_length_c                   11.010(4)
_cell_measurement_reflns_used    2867
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5126
_cell_measurement_theta_min      2.4656
_cell_volume                     2261.9(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Saturn70_(4x4_bin_mode)
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8974
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.9398
_exptl_absorpt_correction_T_min  0.8846
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            cuboid
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    condtr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         4921
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                3972
_reflns_number_total             4921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3000813_si_001.cif
_cod_data_source_block           complex_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2261.8(15)
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C24 H19 Mn N4 O5.50'
_cod_database_code               4506015