Trichloromethyl Chloroformate ("Diphosgene"), ClC(O)OCCl~3~: Structure and Conformational Properties in the Gaseous and Condensed Phases
Valeria B. Arce; Carlos O. Della Védova; Anthony J. Downs; Simon Parsons; Rosana M. Romano; Journal of Organic Chemistry 71 (2006) 3423–3428; doi:10.1021/jo052260a

data_4021652
_publ_section_title
;
 Trichloromethyl Chloroformate ("Diphosgene"), ClC(O)OCCl~3~:
 Structure and Conformational Properties in the Gaseous
 and Condensed Phases
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3423
_journal_page_last               3428
_journal_paper_doi               10.1021/jo052260a
_journal_volume                  71
_journal_year                    2006
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ClC(O)OCl3
_chemical_formula_sum            'C2 Cl4 O2'
_chemical_formula_weight         197.83
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   N/A
_atom_sites_solution_primary     Patterson
_audit_creation_date             02-12-06
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 102.443(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5578(5)
_cell_length_b                   14.2895(12)
_cell_length_c                   8.6246(7)
_cell_measurement_reflns_used    3287
_cell_measurement_temperature    150
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     668.9(1)
_computing_cell_refinement
; 
 SAINT (Siemens ,1995) 
;
_computing_data_collection
; 
 SMART (Siemens, 1993) 
;
_computing_data_reduction
; 
 SAINT (Siemens ,1995) 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 DIRDIF-96 (Beurskens et al 1996) 
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type
; 
Bruker SMART 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1594
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS (Siemens, 1996) 
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' cylinder '
_exptl_crystal_F_000             386.491
_exptl_crystal_size_max          1.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0420
_refine_ls_hydrogen_treatment    N/A
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1482
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.000585
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method= Tukey and Prince 
 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 
 
 1.04 1.09 0.744 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0271
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                1482
_reflns_number_total             1594
_reflns_threshold_expression     >2.00\s(I)
_cod_data_source_file            jo052260asi20060222_050250.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
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 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        ' C2 Cl4 O2 '
_cod_database_code               4021652