Ethyl 5-amino-1-(4-chlorophenyl-5,5-dimethyl-2-oxo-1,3,2-dioxaphosphinan-2-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) o3307–o3309; doi:10.1107/S160053680502917X

data_2207000
_publ_section_title
;Ethyl
 5-amino-1-(4-chlorophenyl-5,5-dimethyl-2-oxo-1,3,2-dioxaphosphinan-2-yl)-3-(6-chloro-3-pyridylmethylamino)-1<i>H</i>-pyrazole-4-carboxylate
;
_journal_coeditor_code           KP6058
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3307
_journal_page_last               o3309
_journal_paper_doi               10.1107/S160053680502917X
_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
;Ethyl
 5-amino-1-(4-chlorophenyl-5,5-dimethyl-2-oxo-1,3,2-dioxaphosphinan-2-yl)-
3-(6-chloro-3-pyridylmethylamino)-1H-pyrazole-4-carboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                86.447(2)
_cell_angle_beta                 85.668(3)
_cell_angle_gamma                70.083(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1968(11)
_cell_length_b                   10.2180(14)
_cell_length_c                   16.581(2)
_cell_measurement_reflns_used    2290
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.72
_cell_volume                     1301.0(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6926
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.9324
_exptl_absorpt_correction_T_min  0.8711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.450
_refine_ls_extinction_coef       0.044(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0711P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                3469
_reflns_number_total             4540
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp6058.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               2207000
_cod_database_fobs_code          2207000