Route towards diselenadiazafulvalenes
Časar, Zdenko; Lorcy, Dominique; Bénard-Rocherullé, Patricia; Majcen-Le Maréchal, Alenka; Chemical Communications  (2001) 1336–; doi:10.1039/b101757h

data_7114729
_publ_section_title
;
 Route towards diselenadiazafulvalenes
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1336
_journal_paper_doi               10.1039/b101757h
_journal_year                    2001
_chemical_formula_moiety         'C16 H14 N2 O Se2'
_chemical_formula_sum            'C16 H14 N2 O Se2'
_chemical_formula_weight         408.21
_chemical_melting_point          193
_chemical_name_common
;
4,3'-dimethyl-4H,3'H-spiro[benzo[1,4]selenazine-2,2'-benzoselenazol']-3-one
;
_chemical_name_systematic
; 
4,3'-dimethyl-4H,3'H-spiro[benzo[1,4]selenazine-2,2'-benzoselenazol']-3-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 98.955(1)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   5.8828(1)
_cell_length_b                   15.9217(5)
_cell_length_c                   16.1883(6)
_cell_measurement_reflns_used    17183
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1497.78(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
'HKL Denzo & Scalepack (Otwinowski & Minor, 1997)'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0267489
_diffrn_orient_matrix_UB_12      -0.1630425
_diffrn_orient_matrix_UB_13      -0.0481113
_diffrn_orient_matrix_UB_21      0.0043632
_diffrn_orient_matrix_UB_22      -0.0170732
_diffrn_orient_matrix_UB_23      0.0602846
_diffrn_orient_matrix_UB_31      -0.0593581
_diffrn_orient_matrix_UB_32      -0.0196385
_diffrn_orient_matrix_UB_33      -0.0012657
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K-alpha'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19344
_diffrn_reflns_theta_full        30.034
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    4.94
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Gaussian integration (Coppens, 1970)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.446
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0611P)^2^+3.0335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                2906
_reflns_number_total             4370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101757h.txt
_cod_data_source_block           num
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7114729