Synthesis and Crystal Structure of 1,4,10,13-Tetraoxa-7,16-diazoniumcyclo- octadecane bis(4-chloro-2-methyl-phenoxyacetate)
Adamovich, S. N.; Mirskova, A. N.; Mirskov, R. G.; Schilde, Uwe; Chemistry Central Journal20115:23 5 (2011) 23–; doi:10.1186/1752-153X-5-23

data_1547205
_publ_section_title
;
 Synthesis and Crystal Structure of
 1,4,10,13-Tetraoxa-7,16-diazoniumcyclo- octadecane
 bis(4-chloro-2-methyl-phenoxyacetate)
;
_journal_name_full               'Chemistry Central Journal20115:23'
_journal_page_first              23
_journal_paper_doi               10.1186/1752-153X-5-23
_journal_volume                  5
_journal_year                    2011
_chemical_formula_moiety         'C6 H14 N O2(+), C9 H8 Cl O3(-)'
_chemical_formula_sum            'C15 H22 Cl N O5'
_chemical_formula_weight         331.79
_chemical_melting_point          401
_chemical_name_systematic
; 
 1,4,10,13-Tetraoxa-7,16-diazoniumcyclo-
 octadecane bis(4-chloro-2-methyl-phenoxyacetate)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                97.624(7)
_cell_angle_beta                 93.340(6)
_cell_angle_gamma                108.945(6)
_cell_formula_units_Z            2
_cell_length_a                   7.5342(6)
_cell_length_b                   9.1935(8)
_cell_length_c                   12.8532(10)
_cell_measurement_reflns_used    8906
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      1.61
_cell_volume                     829.73(12)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-RED (Stoe, 2004)'
_computing_molecular_graphics
;
 ORTEP-3 for Windows (Farrugia, 2005) based on ORTEP-III
 (Burnett & Johnson, 2000)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details
;
 180 frames, detector distance = 140 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, 1.0 \%'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5361
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             352
_exptl_crystal_size_max          1.5
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.11110
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                2280
_reflns_number_total             2738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            13065_2011_284_MOESM1_ESM.CIF
_cod_data_source_block           mir1
_cod_database_code               1547205