Structure of a tricyclo[3.2.1.0^2,7^]octene derivative: a double bridged central ring in an octahydrobenz[<i>g</i>]-3-nitroindole
Meetsma, A.; ten Have, R.; Leusink, F. R.; van Leusen, A. M.; Acta Crystallographica Section C 49 (1993) 826–828; doi:10.1107/S0108270192011156

data_2001829
_publ_contact_author
;
     Meetsma, Auke
     Crystal Structure Center
     Department of Chemical Physics
     University of Groningen
     Nijenborgh 4
     NL-9747 AG Groningen
     The Netherlands
;
_publ_section_title
;
 Structure of a tricyclo[3.2.1.0^2,7^]octene derivative: a double
 bridged central ring in an octahydrobenz[<i>g</i>]-3-nitroindole
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              826
_journal_page_last               828
_journal_paper_doi               10.1107/S0108270192011156
_journal_volume                  49
_journal_year                    1993
_chemical_formula_moiety         'C21 H22 N2 O2'
_chemical_formula_structural     'C21 H22 N2 O2'
_chemical_formula_sum            'C21 H22 N2 O2'
_chemical_formula_weight         334.42
_chemical_melting_point          189.5(5)
_chemical_name_systematic
;
 rac-1-methyl-3-nitro-{(1R,6S,8S)-6-phenyl-5,8-(tetramethylene)tricyclo
 [3.2.1.0^2.7^]oct-3-eno}[4,3-b]pyrrole
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method
;
     spawned by the program PLATON with option: TABLE ACC'
;
_cell_angle_alpha                109.638(4)
_cell_angle_beta                 100.339(6)
_cell_angle_gamma                97.756(6)
_cell_formula_units_Z            2
_cell_length_a                   7.7990(10)
_cell_length_b                   9.8720(10)
_cell_length_c                   11.7700(10)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    130
_cell_measurement_theta_max      18.97
_cell_measurement_theta_min      15.54
_cell_volume                     820.77(16)
_computing_cell_refinement
'CAD-4 version 5.0, SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'CAD-4 version 5.0 (Enraf-Nonius, 1988)'
_computing_data_reduction        'EUCLID (Spek, 1982)'
_computing_molecular_graphics    'PLUTO92 (Meetsma, 1992)'
_computing_publication_material  'PLATON92 (Spek, 1992)'
_computing_structure_refinement  'XTAL_CRYLSQ (Olthof-Hazekamp, 1990)'
_computing_structure_solution    'SHELXS (Sheldrick, 1990)'
_diffrn_ambient_temperature      130
_diffrn_measurement_device
;
      Enraf-Nonius CAD-4F single-crystal diffractometer
;
_diffrn_measurement_method       ' \w/2\q'
_diffrn_radiation_monochromator  'perpendicular mounted graphite'
_diffrn_radiation_source         'fine focus Philips Mo tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_av_sigmaI/netI    0.022
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4098
_diffrn_reflns_reduction_process
;The intensity data were corrected for Lorentz and polarization effects
and
 scale variation but an absorption correction was judged not to be necessary
 in view of the small observed variation in intensity of a 360 \% \y-scan of a
 close-to-axial reflection (-2,0,2).
The variance \s^2^(I) was calculated on
 the basis of counting statistics plus the term (PI)^2^, where P (= 0.021) is
 the instability constant as
derived from the excess variance in the reference
 reflections (McCandlish, Stout & Andrews, 1975). Equivalent reflections were
 averaged and stated observed
if satisfying the criterion I >= 2.5\s(I).
;
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        0.9
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.82
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.392
_refine_ls_abs_structure_details
;
 ?
;
_refine_ls_goodness_of_fit_all   0.725
_refine_ls_goodness_of_fit_obs   0.751
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3265
_refine_ls_R_factor_all          0.051
_refine_ls_R_factor_obs          0.048
_refine_ls_shift/esd_max         0.3840
_refine_ls_shift/esd_mean        0.02455
_refine_ls_structure_factor_coef F~o~
_refine_ls_weighting_details     'w = 1/[\s^2^(F)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.059
_refine_ls_wR_factor_obs         0.058
_reflns_number_observed          3265
_reflns_number_total             3569
_reflns_observed_criterion       I>2.5\s(I)
_cod_data_source_file            ab1037.cif
_cod_data_source_block           CP193
_cod_depositor_comments
;
 Removing duplicate lines from the aniso value loop.

 Antanas Vaitkus,
 2018-05-24

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '189:190' was changed to '189.5(5)' -
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 '189:190' was changed to '189.5(5)' -
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Triclinic' changed to
'triclinic' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(F)]' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w = 1/[\s^2^(F)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        820.77(15)
_cod_database_code               2001829