Crystal structure of diethyl [(4-chloroanilino)(4-hydroxyphenyl)methyl]phosphonate <i>N</i>,<i>N</i>-dimethylformamide monosolvate
Wang, Qing-Ming; Zhu, Ming-Juan; Yang, Jin-Ming; Wang, Shan-Shan; Shang, Yan-Fang; Acta Crystallographica Section E 70 (2014) o919–o920; doi:10.1107/S1600536814016626

data_2239866
_publ_section_title
;
 Crystal structure of diethyl
 [(4-chloroanilino)(4-hydroxyphenyl)methyl]phosphonate
 <i>N</i>,<i>N</i>-dimethylformamide monosolvate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o919
_journal_page_last               o920
_journal_paper_doi               10.1107/S1600536814016626
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C17 H21 Cl N O4 P, C3 H7 N O'
_chemical_formula_moiety         'C17 H21 Cl N O4 P, C3 H7 N O'
_chemical_formula_sum            'C20 H28 Cl N2 O5 P'
_chemical_formula_weight         442.86
_chemical_name_systematic
;
Diethyl [(4-chloroanilino)(4-hydroxyphenyl)methyl]phosphonate
<i>N</i>,<i>N</i>-dimethylformamide monosolvate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.872(2)
_cell_angle_beta                 88.159(2)
_cell_angle_gamma                83.841(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7230(3)
_cell_length_b                   11.6834(5)
_cell_length_c                   13.4582(5)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.65
_cell_volume                     1133.58(8)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17340
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.405
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5126
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0923P)^2^+0.5091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                3982
_reflns_number_total             5126
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz5129sup1.cif
_cod_data_source_block           I
_cod_database_code               2239866
_cod_database_fobs_code          2239866