#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/74/7207491.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7207491
loop_
_publ_author_name
'Yufit, D. S.'
'Howard, J. A. K.'
_publ_section_title
;
 Low melting molecular complexes. The structures of molecular complexes of
 tri- and di-chloromethanes with small ketones and 1,4-dioxane
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              2003
_journal_paper_doi               10.1039/c2ce06526f
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C4 H8 O2, 2 C H2 Cl2'
_chemical_formula_sum            'C6 H12 Cl4 O2'
_chemical_formula_weight         257.96
_chemical_melting_point          205.5(5)
_chemical_name_common            'dichloromethane dioxane co-crystal'
_chemical_name_systematic
;
dichloromethane 1,4-dioxane clathrate (2:1)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
manual editing of the CIF file
created by SHELXTL Ver. 6.14
and processed with modiCIfer-09152005.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8287(13)
_cell_length_b                   10.025(2)
_cell_length_c                   14.764(3)
_cell_measurement_reflns_used    1108
_cell_measurement_temperature    195.0(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      2.76
_cell_volume                     1158.7(4)
_computing_cell_refinement       'SAINT Ver. 6.45 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.630 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.45'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      195.0(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker SMART CCD 6000'
_diffrn_measurement_method       '0.30° ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8652
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.7565
_exptl_absorpt_correction_T_min  0.6940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0076(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                1074
_reflns_number_total             1462
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c2ce06526f.txt
_cod_data_source_block           9_dd1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '205-206' was changed to '205.5(5)' -
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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        1158.8(4)
_cod_original_sg_symbol_Hall     '-P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               7207491
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
O1 O 0.04928(17) 0.48374(13) 0.09089(8) 0.0495(3) Uani 1 1 d
C1 C 0.0434(3) 0.37376(19) 0.02970(14) 0.0518(5) Uani 1 1 d
C2 C 0.0868(3) 0.60305(19) 0.04245(13) 0.0481(4) Uani 1 1 d
H11 H 0.010(3) 0.296(2) 0.0651(14) 0.063(6) Uiso 1 1 d
H12 H 0.153(3) 0.361(2) 0.0012(14) 0.062(6) Uiso 1 1 d
H21 H 0.197(3) 0.596(2) 0.0165(13) 0.050(5) Uiso 1 1 d
H22 H 0.088(3) 0.675(2) 0.0884(14) 0.066(6) Uiso 1 1 d
Cl1 Cl 0.01586(7) 0.47681(5) 0.37443(4) 0.06028(19) Uani 1 1 d
Cl2 Cl 0.18800(10) 0.26370(6) 0.27788(5) 0.0844(3) Uani 1 1 d
C1S C 0.1773(3) 0.43601(19) 0.29593(13) 0.0462(4) Uani 1 1 d
H1S H 0.149(3) 0.475(2) 0.2404(15) 0.053(5) Uiso 1 1 d
H2S H 0.281(3) 0.465(2) 0.3240(14) 0.062(6) Uiso 1 1 d
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0590(8) 0.0540(7) 0.0354(6) 0.0037(5) -0.0022(6) 0.0023(6)
C1 0.0631(13) 0.0411(9) 0.0512(10) 0.0060(8) 0.0052(9) 0.0083(9)
C2 0.0501(12) 0.0468(9) 0.0474(10) -0.0057(8) 0.0064(9) -0.0058(8)
Cl1 0.0573(4) 0.0632(3) 0.0604(3) -0.0054(2) 0.0075(2) 0.0054(2)
Cl2 0.0963(5) 0.0491(3) 0.1078(5) 0.0019(3) 0.0394(4) 0.0094(3)
C1S 0.0488(12) 0.0492(10) 0.0407(9) 0.0042(7) -0.0006(8) -0.0024(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 C1 109.75(14) . . yes
O1 C1 C2 110.73(15) . 5_565 yes
O1 C1 H11 106.6(12) . . ?
C2 C1 H11 109.1(13) 5_565 . ?
O1 C1 H12 110.4(13) . . ?
C2 C1 H12 108.5(13) 5_565 . ?
H11 C1 H12 111.5(18) . . ?
O1 C2 C1 110.40(16) . 5_565 yes
O1 C2 H21 109.1(12) . . ?
C1 C2 H21 110.2(12) 5_565 . ?
O1 C2 H22 105.5(12) . . ?
C1 C2 H22 112.5(13) 5_565 . ?
H21 C2 H22 108.9(18) . . ?
Cl2 C1S Cl1 111.32(11) . . yes
Cl2 C1S H1S 107.0(12) . . ?
Cl1 C1S H1S 108.1(13) . . ?
Cl2 C1S H2S 109.0(13) . . ?
Cl1 C1S H2S 104.7(13) . . ?
H1S C1S H2S 116.7(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.424(2) . yes
O1 C1 1.426(2) . yes
C1 C2 1.492(3) 5_565 yes
C1 H11 0.97(2) . ?
C1 H12 0.97(2) . ?
C2 C1 1.492(3) 5_565 yes
C2 H21 0.95(2) . ?
C2 H22 0.99(2) . ?
Cl1 C1S 1.763(2) . yes
Cl2 C1S 1.750(2) . yes
C1S H1S 0.93(2) . ?
C1S H2S 0.96(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1S H1S O1 0.93(2) 2.34(2) 3.225(2) 156.8(17) .
C1S H2S O1 0.96(2) 2.45(2) 3.391(3) 166.1(18) 6_656
