A Representative of P,P,P-Trihalogenylides: Synthesis and Structure
Anatoliy P. Marchenko; Georgyi N. Koidan; Aleksandr N. Kostyuk; Andrei A. Tolmachev; Evgenij G. Kapustin; Aleksandr M. Pinchuk; Journal of Organic Chemistry 71 (2006) 8633–8636; doi:10.1021/jo0606352

data_4022027
_publ_contact_author             'Rusanov, Eduard B.'
_publ_contact_author_email       rusanov@bpci.kiev.ua
_publ_section_title
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 A Representative of P,P,P-Trihalogenylides: Synthesis and Structure
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8633
_journal_page_last               8636
_journal_paper_doi               10.1021/jo0606352
_journal_volume                  71
_journal_year                    2006
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C10 H8 Cl3 N2 O1 P1 '
_chemical_formula_sum            'C10 H8 Cl3 N2 O P'
_chemical_formula_weight         309.52
_chemical_melting_point          390
_chemical_name_systematic
;                                                                               
5-methyl-2-phenyl-4-(trichlorophoshoranylidene)-
2,4-dihydro-3H-pyrazol-3-one
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.028(4)
_cell_length_b                   12.923(5)
_cell_length_c                   16.482(4)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293
_cell_measurement_theta_max      23
_cell_measurement_theta_min      20
_cell_volume                     2561.8(14)
_computing_cell_refinement
; 
 Cad4 Express, (Enraf-Nonius, 1989) 
;
_computing_data_collection
; 
 Cad4 Express, (Enraf-Nonius, 1989) 
;
_computing_data_reduction
; 
 RC93 (Watkin, Prout & Lilley, 1994) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type
; 
Enraf-Nonius CAD-4 
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2580
_diffrn_reflns_theta_full        51.962
_diffrn_reflns_theta_max         67.924
_diffrn_reflns_theta_min         5.368
_diffrn_standards_decay_%        3.29
_diffrn_standards_interval_count 147
_diffrn_standards_interval_time  '3600 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.543
_exptl_absorpt_correction_T_max  0.05
_exptl_absorpt_correction_T_min  0.01
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al, 1968) 
;
_exptl_crystal_colour            ' light-green '
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1248.000
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.49
_refine_ls_extinction_coef       25.606
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.1512
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         933
_refine_ls_R_factor_all          0.1734
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.004368
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1308
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0625
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                933
_reflns_number_total             2272
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            jo0606352si20060323_101421.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        ' C10 H8 Cl3 N2 O1 P1 '
_cod_database_code               4022027
_refine_ls_r_factor_ref          0.0612