3-(Dimethylamino)-5,6,7,8,9,10-hexahydro-12,13-dimethoxy-4<i>H</i>-spiro[benzo-1-thia-2,5-diazacyclododecene-4,1'-cyclobutan]-6-one 1,1-Dioxide Dichloromethane Solvate (1/1) at 173K
Linden, Anthony; Mihova, Tonya R.; Heimgartner, Heinz; Acta Crystallographica Section C 54 (1998) 1659–1662; doi:10.1107/S0108270198008476

data_2007811
_publ_section_title
;3-(Dimethylamino)-5,6,7,8,9,10-hexahydro-12,13-dimethoxy-4<i>H</i>-spiro[benzo-1-thia-2,5-diazacyclododecene-4,1'-cyclobutan]-6-one
 1,1-Dioxide Dichloromethane Solvate (1/1) at 173K
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1659
_journal_page_last               1662
_journal_paper_doi               10.1107/S0108270198008476
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C20 H29 N3 O5 S, C H2 Cl2'
_chemical_formula_sum            'C21 H31 Cl2 N3 O5 S'
_chemical_formula_weight         508.46
_chemical_melting_point          250(5)
_chemical_name_systematic
;3-(dimethylamino)-5,6,7,8,9,10-hexahydro-12,13-dimethoxy-4H-spiro[benzo-1-thia-2
,5-diazacyclododecene-4,1'-cyclobutan]-6-one
 1,1-dioxide dichloromethane
solvate (1/1)
;
_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           SHELXL-97
_cell_angle_alpha                97.72(2)
_cell_angle_beta                 102.21(2)
_cell_angle_gamma                102.980(10)
_cell_formula_units_Z            2
_cell_length_a                   12.112(2)
_cell_length_b                   13.460(2)
_cell_length_c                   7.946(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      18.5
_cell_volume                     1211.1(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1991)
;
_computing_data_reduction
'TEXSAN PROCESS (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'SHELXS86 (direct methods) (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-5R diffractometer'
_diffrn_measurement_method       '\w--2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode generator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5827
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        insignificant
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment
'H atoms treated by a mixture of independent and constrained refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5565
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0602P)^2^+1.4198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                3797
_reflns_number_total             5565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fg1482.cif
_cod_data_source_block           hg9816
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '244.7-255.1' was changed to '250(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 '244.7-255.1' was changed to '250(5)'
- 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_original_sg_symbol_H-M      P-1
_cod_database_code               2007811
_cod_database_fobs_code          2007811