data_2001545
_journal_name_full 'Acta Crystallographica, Section C'
_journal_year 1993
_journal_volume C49
_journal_page_first 1376
_journal_page_last 1378
_publ_section_title
;
Structure of the Benzo-15-crown-5--3,5-Dinitrobenzoic Acid--
Water (1/1/1) Complex
;
loop_
_publ_author_name
'Schouten*, A. '
'Kanters, J.A.'
'Poonia, N.S.'
_chemical_name_systematic
;
(3,5-dinitrobenzoic acid)(benzo-15-crown-5)monohydrate
;
_chemical_formula_moiety 'C7 H4 N2 O6, C14 H20 O5, H2 O'
_chemical_formula_sum 'C21 H26 N2 O12'
_chemical_formula_weight 498.44
_chemical_melting_point 373.0(5)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21'
loop_
_symmetry_equiv_pos_as_xyz
'+x,+y, +z'
'-x, 1/2+y, -z'
_cell_length_a 7.0711(4)
_cell_length_b 15.0900(10)
_cell_length_c 11.1925(6)
_cell_angle_alpha 90
_cell_angle_beta 106.916(4)
_cell_angle_gamma 90
_cell_volume 1142.60(12)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 10.62
_cell_measurement_theta_max 17.51
_cell_measurement_temperature 100
_exptl_crystal_description rod
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.78
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.17
_exptl_crystal_density_diffrn 1.449
_exptl_crystal_density_meas ?
_exptl_crystal_F_000 524
_exptl_absorpt_coefficient_mu 0.113
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_diffrn_ambient_temperature 100
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_monochromator 'Zr filter'
_diffrn_measurement_device 'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method \w/2\q
_diffrn_reflns_number 6772
_diffrn_reflns_av_R_equivalents 0.041
_diffrn_reflns_av_sigmaI/netI 0.0198
_diffrn_reflns_theta_min 1.35
_diffrn_reflns_theta_max 30.26
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 0
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_standards_number 3
_diffrn_standards_interval_time 60
_diffrn_standards_decay_% 2.3
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 2 2
-2 1 0
-1 0 -2
_reflns_number_total 3413
_reflns_number_observed 2992
_reflns_observed_criterion '>2.5sigma(I)'
_refine_ls_structure_factor_coef F
_refine_ls_matrix_type full
_refine_ls_R_factor_obs 0.0332
_refine_ls_wR_factor_obs 0.0297
_refine_ls_goodness_of_fit_obs 1.49
_refine_ls_number_reflns 2992
_refine_ls_number_parameters 420
_refine_ls_number_restraints ?
_refine_ls_number_constraints ?
_refine_ls_hydrogen_treatment refall
_refine_ls_weighting_scheme 'w = 1/[\s^2^(F)]'
_refine_ls_shift/esd_max 0.037
_refine_ls_shift/esd_mean 0.0050
_refine_diff_density_max 0.27
_refine_diff_density_min -0.26
_refine_ls_extinction_method SHELX76
_refine_ls_extinction_coef 0.0016
_refine_ls_abs_structure_details
;
;
_refine_ls_abs_structure_Flack ?
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.002 0.002 International_Tables_Vol_IV_Table_2.2B
H 0 0 International_Tables_Vol_IV_Table_2.2B
N 0.004 0.003 International_Tables_Vol_IV_Table_2.2B
O 0.008 0.006 International_Tables_Vol_IV_Table_2.2B
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
O7 0.7759(2) 0.1483(2) 0.85950(10)
 0.0165(4) Uani
O8 0.9036(2) 0.0920(2) 1.10660(10)
 0.0201(4) Uani
O9 0.7704(2) 0.2561(2) 1.20360(10)
 0.0222(5) Uani
O10 0.8236(2) 0.4062(2) 1.05740(10)
  0.0203(4) Uani
O11 0.7285(2) 0.3141(2) 0.83120(10)
  0.0167(4) Uani
C8 0.8208(3) 0.1279(2) 0.6531(2) 0.0173(6) Uani
C9 0.7891(3) 0.1795(2) 0.7476(2) 0.0148(5) Uani
C10 0.7624(3) 0.2714(2) 0.7320(2) 0.0145(5) Uani
C11 0.7659(3) 0.3108(2) 0.6204(2) 0.0191(6) Uani
C12 0.7939(3) 0.2578(2) 0.5236(2) 0.0200(6) Uani
C13 0.8213(3) 0.1683(2) 0.5400(2) 0.0204(6) Uani
C14 0.8237(3) 0.0574(2) 0.8892(2) 0.0189(6) Uani
C15 0.7750(3) 0.0410(2) 1.0091(2) 0.0200(6) Uani
C16 0.8293(4) 0.1011(2) 1.2125(2) 0.0230(6) Uani
C17 0.6742(3) 0.1724(2) 1.1962(2) 0.0223(6) Uani
C18 0.6354(3) 0.3284(2) 1.1757(2) 0.0247(6) Uani
C19 0.7501(4) 0.4103(2) 1.1639(2) 0.0237(6) Uani
C20 0.6815(4) 0.4375(2) 0.9465(2) 0.0219(6) Uani
C21 0.7379(3) 0.4089(2) 0.8334(2) 0.0197(6) Uani
O1 1.3613(3) 0.0807(2) 0.3648(2) 0.0354(6) Uani
O2 1.3940(3) 0.0041(2) 0.5335(2) 0.0355(5) Uani
O3 1.2881(2) 0.1395(2) 0.90410(10)
 0.0237(4) Uani
O4 1.2216(2) 0.2852(2) 0.89890(10)
 0.0209(4) Uani
O5 1.1720(3) 0.4538(2) 0.5268(2) 0.0466(8) Uani
O6 1.2328(3) 0.3946(2) 0.36590(10)
 0.0312(5) Uani
N1 1.3635(3) 0.0736(2) 0.4745(2) 0.0264(6) Uani
N2 1.2203(3) 0.3911(2) 0.4725(2) 0.0251(6) Uani
C1 1.2955(3) 0.23311 0.4740(2) 0.0189(6) Uani
C2 1.3267(3) 0.1542(2) 0.5389(2) 0.0195(6) Uani
C3 1.3228(3) 0.1465(2) 0.6614(2) 0.0181(6) Uani
C4 1.2849(3) 0.2215(2) 0.7227(2) 0.0156(5) Uani
C5 1.2533(3) 0.3026(2) 0.6615(2) 0.0167(6) Uani
C6 1.2602(3) 0.3060(2) 0.5391(2) 0.0189(6) Uani
C7 1.2673(3) 0.2111(2) 0.8522(2) 0.0174(6) Uani
O22 1.1016(2) 0.2578(2) 1.0873(2) 0.0238(5) Uani
H81 0.841(3) 0.066(2) 0.669(2) 0.015(5) Uiso
H111 0.748(3) 0.3730(10)
   0.613(2) 0.013(5) Uiso
H121 0.791(4) 0.285(2) 0.452(2) 0.024(6) Uiso
H131 0.843(3) 0.131(2) 0.476(2) 0.024(6) Uiso
H141 0.968(3) 0.0500(10)
   0.896(2) 0.016(6) Uiso
H142 0.751(4) 0.021(2) 0.826(2) 0.021(6) Uiso
H151 0.793(3) -0.019(2) 1.028(2) 0.022(6) Uiso
H152 0.637(3) 0.0600(10)
   1.001(2) 0.010(5) Uiso
H161 0.770(4) 0.046(2) 1.231(2) 0.024(6) Uiso
H162 0.940(4) 0.112(2) 1.278(2) 0.020(6) Uiso
H171 0.574(3) 0.1650(10)
   1.115(2) 0.016(5) Uiso
H172 0.611(4) 0.171(2) 1.267(2) 0.029(6) Uiso
H181 0.526(3) 0.314(2) 1.091(2) 0.021(6) Uiso
H182 0.576(3) 0.337(2) 1.243(2) 0.027(6) Uiso
H191 0.863(4) 0.414(2) 1.233(2) 0.029(7) Uiso
H192 0.679(3) 0.461(2) 1.160(2) 0.015(6) Uiso
H201 0.675(3) 0.503(2) 0.949(2) 0.018(6) Uiso
H202 0.548(3) 0.410(2) 0.939(2) 0.021(6) Uiso
H211 0.868(4) 0.426(2) 0.836(2) 0.021(6) Uiso
H212 0.641(3) 0.4350(10)
   0.759(2) 0.016(6) Uiso
H11 1.293(3) 0.237(2) 0.386(2) 0.021(6) Uiso
H31 1.341(3) 0.091(2) 0.703(2) 0.011(5) Uiso
H41 1.187(4) 0.272(2) 0.960(2) 0.029(7) Uiso
H51 1.222(3) 0.355(2) 0.699(2) 0.022(6) Uiso
H221 1.009(4) 0.294(2) 1.084(2) 0.039(8) Uiso
H222 1.044(5) 0.212(3) 1.083(3) 0.060(10)
Uiso