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_4506016
_publ_section_title
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 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            'C49 H38 Mn2 N8 O10'
_chemical_formula_weight         1008.75
_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                85.114(11)
_cell_angle_beta                 84.884(11)
_cell_angle_gamma                80.510(13)
_cell_formula_units_Z            2
_cell_length_a                   9.928(5)
_cell_length_b                   13.554(7)
_cell_length_c                   17.063(9)
_cell_measurement_reflns_used    4373
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5711
_cell_measurement_theta_min      3.0037
_cell_volume                     2250(2)
_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 14.6306
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  Mercury70_(2x2_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  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31706
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.7861
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelike
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         10289
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0672
_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 w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+2.7961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1758
_reflns_number_gt                7139
_reflns_number_total             10289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg3000813_si_001.cif
_cod_data_source_block           complex_6
_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_sg_symbol_H-M      P-1
_cod_database_code               4506016