(+/-)-(3'aα,4'α,6'aα)-3',3'a,4',6'a-Tetrahydro-5,5,<i>N</i>,<i>N</i>-tetramethylspiro[1,3-dioxane-2,2'(1'<i>H</i>)-pentalene]-4'-acetamide, a triclinic crystal structure with local monoclinic pseudosymmetry
Jan W. Bats; Öhlinger, Stefan H.; Mulzer, Johann; Acta Crystallographica Section C 55 (1999) 1158–1160; doi:10.1107/S0108270199003765

data_2008692
_publ_section_title
;(+/-)-(3'a\a,4'\a,6'a\a)-3',3'a,4',6'a-Tetrahydro-5,5,<i>N</i>,<i>N</i>-tetramethylspiro[1,3-dioxane-2,2'(1'<i>H</i>)-pentalene]-4'-acetamide,
 a triclinic crystal structure with local monoclinic pseudosymmetry
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1158
_journal_page_last               1160
_journal_paper_doi               10.1107/S0108270199003765
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C17 H27 N O3'
_chemical_formula_weight         293.41
_chemical_name_systematic
;
(+-)-(3'a\a,4'\b,6'a\a)-1',3',3'a,6'a-Tetrahydro-5,5,N,N-
tetramethyl-spiro[1,3-dioxane-2,2'(1'H)-pentalene]-4'-
acetamide
;
_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_type_scat_source
International_Tables_for_Xray_Crystallography_(Vol._IV)
_cell_angle_alpha                104.889(12)
_cell_angle_beta                 96.663(12)
_cell_angle_gamma                90.451(9)
_cell_formula_units_Z            4
_cell_length_a                   9.4850(13)
_cell_length_b                   11.769(2)
_cell_length_c                   14.596(2)
_cell_measurement_reflns_used    213
_cell_measurement_temperature    135
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     1562.8(4)
_computing_cell_refinement       SMART
_computing_data_collection       SMART_(Siemens,_1995)
_computing_data_reduction        SAINT_(Siemens,_1995)
_computing_molecular_graphics    XP_in_SHELXTL
_computing_publication_material  CIF_in_MolEN
_computing_structure_refinement  LSFM_in_MolEN_(Fair,_1990)
_computing_structure_solution    Direct_methods_(SHELXTL,_Sheldrick,_1996)
_diffrn_measurement_device       Siemens_SMART
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24913
_diffrn_reflns_theta_max         29.85
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  540
_diffrn_standards_number         332
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   numerical:
_exptl_absorpt_process_details
;
a numerical absorption correction was made based on six indexed
crystal faces using program SHELXTL (Sheldrick, 1996).
;
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          1.02
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.4322
_refine_diff_density_min         -0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    H_atoms_refined_isotropically
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7473
_refine_ls_R_factor_obs          0.056
_refine_ls_shift/su_max          0.015
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/[\s^2^(Fo^2^) + 0.0009Fo^4^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.052
_reflns_number_observed          7473
_reflns_number_total             7688
_reflns_observed_criterion       I>0.0\s(I)
_cod_data_source_file            ka1316.cif
_cod_data_source_block           s0203
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/[\s^2^(Fo^2^) +
0.0009Fo^4^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 4Fo^2^/[\s^2^(Fo^2^) + 0.0009Fo^4^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        C17H27NO3
_cod_database_code               2008692