Diethyl 2,8-diamino-4,10-bis(3-nitrophenyl)naphtho[1,2-<i>b</i>;6,5-<i>b</i>']dipyran-3,9-dicarboxylate dimethylformamide disolvate
Yu-Cheng Wang; Xiang-Shan Wang; Zhao-Sen Zeng; Da-Qing Shi; Acta Crystallographica Section E 61 (2005) o2027–o2029; doi:10.1107/S1600536805017113

data_2206254
_publ_section_title
;Diethyl
 2,8-diamino-4,10-bis(3-nitrophenyl)naphtho[1,2-<i>b</i>;6,5-<i>b</i>']dipyran-3,9-dicarboxylate
 dimethylformamide disolvate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2027
_journal_page_last               o2029
_journal_paper_doi               10.1107/S1600536805017113
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C34 H28 N4 O10 , 2C3 H7 N O'
_chemical_formula_moiety         'C34 H28 N4 O10 , 2C3 H7 N O'
_chemical_formula_sum            'C40 H42 N6 O12'
_chemical_formula_weight         798.80
_chemical_melting_point          560.0(10)
_chemical_name_systematic
;
Diethyl 2,8-diamino-4,10-bis(3-nitrophenyl)naphtha[1,2-b;6,5-b']dipyran-
3,9-dicarboxylate dimethylformamide disolvate
;
_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
_cell_angle_alpha                99.292(3)
_cell_angle_beta                 96.912(3)
_cell_angle_gamma                97.103(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3550(10)
_cell_length_b                   9.7500(10)
_cell_length_c                   12.202(2)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    289(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      3.26
_cell_volume                     963.4(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      289(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5054
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        2.26
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.315
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0707
_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^)+(0.16P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2415
_reflns_number_gt                2241
_reflns_number_total             3340
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6529.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '559-561' was changed to '560.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '559-561' was changed to '560.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2206254
_cod_database_fobs_code          2206254