Synthesis of 12,12'-azo-13,13'-diepi-Ritterazine N.
Shi, Yong; Jiang, Xiao-Ling; Tian, Wei-Sheng; The Journal of organic chemistry 82 (2017) 269–275; doi:10.1021/acs.joc.6b02391

data_4032099
_publ_section_title
;
 Synthesis of 12,12'-azo-13,13'-diepi-Ritterazine N.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              269
_journal_page_last               275
_journal_paper_doi               10.1021/acs.joc.6b02391
_journal_volume                  82
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C55.5 H81 N2 O8.5'
_chemical_formula_weight         912.22
_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                 112.568(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.807(3)
_cell_length_b                   16.852(3)
_cell_length_c                   13.0310(14)
_cell_measurement_reflns_used    4922
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.847
_cell_measurement_theta_min      4.965
_cell_volume                     5233.2(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14855
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07710
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.7(12)
_refine_ls_extinction_coef       0.0039(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9343
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1878
_reflns_number_gt                7248
_reflns_number_total             9343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b02391_si_002.cif
_cod_data_source_block           cd213175
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4032099.cif.
;
_cod_original_cell_volume        5233.3(11)
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C55.50 H81 N2 O8.50'
_cod_database_code               4032099