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_4022026
_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_formula_moiety         'C13 H17 N2 O P'
_chemical_formula_sum            'C13 H17 N2 O P'
_chemical_formula_weight         248.26
_chemical_melting_point          460
_chemical_name_systematic
;
5-Methyl-2-phenyl-4-(trimethylphosphoranylidene)-2,4-
dihydro-3H-pyrazol-3-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2005-07-06T18:29:16-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 111.21(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.987(4)
_cell_length_b                   11.679(2)
_cell_length_c                   13.663(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.81
_cell_measurement_theta_min      25.8
_cell_volume                     2675.8(10)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4191
_diffrn_reflns_theta_full        59.97
_diffrn_reflns_theta_max         59.97
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 147
_diffrn_standards_interval_time  '4500 sec.'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.707
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         3952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.086
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.134
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                2780
_reflns_number_total             3952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0606352si20060323_101405.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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4022026