data_7000017
_journal_name_full               'Dalton Trans.'
_journal_year                    2005
_publ_section_title
;
A study of the complexation and extraction of Cu(II)
sulfate and Ni(II) sulfate by N3O2-donor macrocycles
;
loop_
_publ_author_name
'Leonard F. Lindoy'
'Stuart G. Galbraith'
'Vesna Gasperov'
'Brendan R. Rumbel'
'Brian W. Skelton'
'Allan H. White'
_chemical_formula_sum            'C21 H31 Cl2 Cu1 N3 O12'
_chemical_formula_weight         651.94
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  -p_2ybc
loop_
_symmetry_equiv_pos_as_xyz
'+x,+y,+z'
'-x,1/2+y,1/2-z'
'-x,-y,-z'
'+x,1/2-y,1/2+z'
_cell_length_a                   16.921(2)
_cell_length_b                   10.6010(10)
_cell_length_c                   16.233(2)
_cell_angle_alpha                90.00000
_cell_angle_beta                 111.143(2)
_cell_angle_gamma                90.00000
_cell_volume                     2715.9(5)
_cell_formula_units_Z            4
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_cell_measurement_reflns_used    7253
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      28.5
_cell_measurement_temperature    159(2)
_exptl_absorpt_coefficient_mu    1.067
_exptl_crystal_description       prism
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .15
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            blue
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_absorpt_correction_T_min  .661
_exptl_absorpt_correction_T_max  .914
_diffrn_reflns_number            31835
_reflns_number_total             6946
_reflns_Friedel_coverage         0
_reflns_number_gt                4773
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_diffrn_reflns_theta_max         29.
_diffrn_reflns_theta_full        29.
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measured_fraction_theta_full 1.0
_diffrn_reflns_av_R_equivalents  .061
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           .054
_refine_ls_wR_factor_ref         .059
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_number_reflns         4773
_refine_ls_number_parameters     365
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    noref
_refine_ls_shift/su_max          .013
_refine_diff_density_min         -.48
_refine_diff_density_max         .986
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 84 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 124 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 48 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 .29775(3) .17201(4) .21953(3) .0273(2) Uani ? ? 1.00000 ? ?
Cl1 .16681(7) .01706(9) .43216(6) .0376(5) Uani ? ? 1.00000 ? ?
O101 .1690(2) .1424(3) .4655(2) .069(2) Uani ? ? 1.00000 ? ?
O102 .1328(7) -.0684(6) .4685(7) .146(7) Uani ? ? .753(9) ? ?
O103 .2560(3) -.0187(5) .4532(3) .071(3) Uani ? ? .753(9) ? ?
O104 .1333(6) .0181(7) .3394(3) .116(5) Uani ? ? .753(9) ? ?
O102' .2076(12) -.0787(15) .4912(11) .068(5) Uiso ? ? .247(9) ? ?
O103' .1873(12) .0165(18) .3594(13) .069(6) Uiso ? ? .247(9) ? ?
O104' .0746(12) -.009(2) .3990(13) .089(7) Uiso ? ? .247(9) ? ?
Cl2 .50727(6) .14266(8) .15841(6) .0320(4) Uani ? ? 1.00000 ? ?
O201 .42578(17) .1803(3) .1589(2) .0440(15) Uani ? ? 1.00000 ? ?
O202 .5200(2) .1945(3) .08297(19) .0483(16) Uani ? ? 1.00000 ? ?
O203 .5119(2) .0086(3) .1585(2) .0555(17) Uani ? ? 1.00000 ? ?
O204 .57149(18) .1909(3) .23743(19) .0463(15) Uani ? ? 1.00000 ? ?
O1 .26529(18) .3194(2) .14214(17) .0392(13) Uani ? ? 1.00000 ? ?
N1 .3220(2) .0181(3) .2966(2) .0316(14) Uani ? ? 1.00000 ? ?
C2 .4134(3) .0015(4) .3483(3) .0392(19) Uani ? ? 1.00000 ? ?
C3 .4493(3) .1082(4) .4134(3) .039(2) Uani ? ? 1.00000 ? ?
C4 .4486(3) .2363(4) .3710(2) .0334(18) Uani ? ? 1.00000 ? ?
N5 .3608(2) .2846(3) .3239(2) .0291(14) Uani ? ? 1.00000 ? ?
C6 .3181(3) .3165(4) .3887(2) .0330(18) Uani ? ? 1.00000 ? ?
C7 .2753(3) .4409(3) .3702(3) .0321(18) Uani ? ? 1.00000 ? ?
C71 .3128(3) .5468(4) .4173(3) .039(2) Uani ? ? 1.00000 ? ?
C72 .2739(3) .6641(4) .4010(3) .044(2) Uani ? ? 1.00000 ? ?
C73 .1957(3) .6745(4) .3337(3) .047(2) Uani ? ? 1.00000 ? ?
C74 .1562(3) .5712(4) .2837(3) .039(2) Uani ? ? 1.00000 ? ?
C8 .1958(3) .4536(3) .3030(3) .0358(19) Uani ? ? 1.00000 ? ?
O9 .16113(18) .3433(2) .26188(18) .0381(13) Uani ? ? 1.00000 ? ?
C10 .0800(3) .3473(4) .1917(3) .040(2) Uani ? ? 1.00000 ? ?
C11 .0476(3) .2154(4) .1766(3) .038(2) Uani ? ? 1.00000 ? ?
O12 .10109(17) .1456(2) .14180(17) .0337(13) Uani ? ? 1.00000 ? ?
C13 .0783(2) .0230(3) .1182(2) .0302(17) Uani ? ? 1.00000 ? ?
C131 .0176(3) -.0425(4) .1397(3) .036(2) Uani ? ? 1.00000 ? ?
C132 .0006(3) -.1676(4) .1142(3) .040(2) Uani ? ? 1.00000 ? ?
C133 .0435(3) -.2274(4) .0674(3) .039(2) Uani ? ? 1.00000 ? ?
C134 .1034(2) -.1606(3) .0446(2) .0335(18) Uani ? ? 1.00000 ? ?
C14 .1211(2) -.0348(3) .0691(2) .0283(16) Uani ? ? 1.00000 ? ?
C15 .1839(2) .0383(3) .0429(2) .0293(16) Uani ? ? 1.00000 ? ?
N16 .2690(2) .0493(3) .1150(2) .0286(14) Uani ? ? 1.00000 ? ?
C17 .3047(2) -.0745(3) .1541(3) .0317(17) Uani ? ? 1.00000 ? ?
C18 .2870(3) -.0921(3) .2383(3) .0336(18) Uani ? ? 1.00000 ? ?
O301 .3655(2) .5036(3) .1275(2) .075(2) Uani ? ? 1.00000 ? ?
H1 .28833 .02307 .33409 .03900 Uiso ? ? 1.00000 ? ?
H2a .44423 .00221 .30778 .05000 Uiso ? ? 1.00000 ? ?
H2b .42416 -.07722 .37809 .05000 Uiso ? ? 1.00000 ? ?
H3a .50565 .08760 .45236 .05100 Uiso ? ? 1.00000 ? ?
H3b .41475 .11384 .45024 .05100 Uiso ? ? 1.00000 ? ?
H4a .47696 .22794 .32969 .04100 Uiso ? ? 1.00000 ? ?
H4b .47963 .29604 .41525 .04100 Uiso ? ? 1.00000 ? ?
H5 .37921 .36321 .31178 .03600 Uiso ? ? 1.00000 ? ?
H6a .35896 .31738 .44715 .04100 Uiso ? ? 1.00000 ? ?
H6b .27674 .25257 .38536 .04100 Uiso ? ? 1.00000 ? ?
H71 .36796 .53898 .46317 .04900 Uiso ? ? 1.00000 ? ?
H72 .30176 .73664 .43654 .05300 Uiso ? ? 1.00000 ? ?
H73 .16795 .75433 .31994 .05900 Uiso ? ? 1.00000 ? ?
H74 .10167 .58029 .23597 .04900 Uiso ? ? 1.00000 ? ?
H10a .08637 .37908 .13778 .04900 Uiso ? ? 1.00000 ? ?
H10b .04230 .40313 .20518 .04900 Uiso ? ? 1.00000 ? ?
H11a -.01099 .21292 .13665 .04500 Uiso ? ? 1.00000 ? ?
H11b .04869 .17923 .23177 .04500 Uiso ? ? 1.00000 ? ?
H131 -.01293 -.00122 .17150 .04500 Uiso ? ? 1.00000 ? ?
H132 -.04210 -.21295 .12966 .04600 Uiso ? ? 1.00000 ? ?
H133 .03002 -.31435 .04902 .05100 Uiso ? ? 1.00000 ? ?
H134 .13545 -.20286 .01317 .04200 Uiso ? ? 1.00000 ? ?
H15a .16192 .12315 .02644 .03600 Uiso ? ? 1.00000 ? ?
H15b .18992 .00058 -.00761 .03600 Uiso ? ? 1.00000 ? ?
H16 .31167 .08433 .09221 .03300 Uiso ? ? 1.00000 ? ?
H17a .36501 -.07646 .16668 .03800 Uiso ? ? 1.00000 ? ?
H17b .27987 -.14107 .11230 .03800 Uiso ? ? 1.00000 ? ?
H18a .22633 -.09797 .22383 .04200 Uiso ? ? 1.00000 ? ?
H18b .31166 -.16849 .26729 .04200 Uiso ? ? 1.00000 ? ?
H1a .29893 .38588 .14512 .05700 Uiso ? ? 1.00000 ? ?
H1b .22211 .31901 .09247 .05700 Uiso ? ? 1.00000 ? ?