Supramolecular structures of 5-[3-(4-methylphenyl)- and 5-[3-(4-chlorophenyl)-2-propenylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione
Low, John Nicolson; Cobo, Justo; Nogueras, Manuel; Sánchez, Adolfo; Insuasty, Braulio; Torres, Harlen; Acta Crystallographica Section C 58 (2002) o39–o41; doi:10.1107/S0108270101018765

data_2012462
_publ_section_title
;
 Supramolecular structures of 5-[3-(4-methylphenyl)- and
 5-[3-(4-chlorophenyl)-2-propenylidene]-2,2-dimethyl-1,3-dioxane-4,6-dione
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o39
_journal_page_last               o41
_journal_paper_doi               10.1107/S0108270101018765
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C15 H13 Cl O4'
_chemical_formula_sum            'C15 H13 Cl O4'
_chemical_formula_weight         292.70
_chemical_melting_point          455
_chemical_name_systematic
;
5-(3-(4-chlorophenyl)-2-propenylidene]-2,2-dimethyl-[1,3]
dioxane-4,6-dione
;
_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                90.1799(13)
_cell_angle_beta                 99.8452(14)
_cell_angle_gamma                109.576(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2648(2)
_cell_length_b                   7.4705(3)
_cell_length_c                   13.5855(6)
_cell_measurement_reflns_used    3057
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.03
_cell_volume                     683.01(5)
_computing_cell_refinement       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        'Kappa-CCD server software (Nonius, 1997)'
_computing_molecular_graphics
'NRCVAX-96, ORTEP (Johnson, 1976), PLATON (Spek, 2001)'
_computing_publication_material
' SHELXL-97  and WordPerfect macro PRPKAPPA (Ferguson, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_measured_fraction_theta_full .973
_diffrn_measured_fraction_theta_max .970
_diffrn_measurement_device_type  Kappa-CCD
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .077
_diffrn_reflns_av_sigmaI/netI    .0705
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9407
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    .289
_exptl_absorpt_correction_T_max  .9716
_exptl_absorpt_correction_T_min  .9579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .10
_refine_diff_density_max         .617
_refine_diff_density_min         -.664
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .982
_refine_ls_R_factor_all          .0762
_refine_ls_R_factor_gt           .0525
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0932P)^2^+0.2802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .1345
_refine_ls_wR_factor_ref         .1531
_reflns_number_gt                2350
_reflns_number_total             3057
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            sk1522.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '455K' was changed to '455' - the
value should be numeric and without a unit designator.

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 '455K' was changed to '455' - the
value should be numeric and without a unit
designator.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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 
;
_cod_original_cell_volume        683.01(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2012462
_cod_database_fobs_code          2012462