<i>cis</i>-Ethyl 5-amino-1-[4-(4-chlorophenyl)-5,5-dimethyl-2-oxo-1,3,2-dioxaphosphinan-1-yl]-3-(6-chloro-3-pyridylmethylamino)-1<i>H</i>-pyrazole-4-carboxylate
Zai-Gang Luo; De-Qing Shi; Xiang-Gao Meng; Acta Crystallographica Section E 61 (2005) o3679–o3681; doi:10.1107/S1600536805032484

data_2207181
_publ_section_title
;<i>cis</i>-Ethyl
 5-amino-1-[4-(4-chlorophenyl)-5,5-dimethyl-2-oxo-1,3,2-dioxaphosphinan-1-yl]-3-(6-chloro-3-pyridylmethylamino)-1<i>H</i>-pyrazole-4-carboxylate
;
_journal_coeditor_code           CI6662
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3679
_journal_page_last               o3681
_journal_paper_doi               10.1107/S1600536805032484
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C23 H26 Cl2 N5 O5 P'
_chemical_formula_moiety         'C23 H26 Cl2 N5 O5 P'
_chemical_formula_sum            'C23 H26 Cl2 N5 O5 P'
_chemical_formula_weight         554.36
_chemical_name_systematic
;cis-Ethyl
5-amino-1-[4-chlorophenyl-3-(6-chloro-3-pyridylmethylamino)-5,5-dimethyl-2-oxo-
1,3,2-dioxaphosphinan-1-yl]pyrazole-4-carboxylate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.198(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4196(11)
_cell_length_b                   12.1995(11)
_cell_length_c                   17.5992(15)
_cell_measurement_reflns_used    5782
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      22.87
_cell_measurement_theta_min      2.39
_cell_volume                     2547.3(4)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21527
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.8991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                3999
_reflns_number_total             5812
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6662.cif
_cod_data_source_block           I
_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:

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2207181
_cod_database_fobs_code          2207181