#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:39:42 +0100 (vie 25 de mar de 2016) $
#$Revision: 179801 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/97/7009783.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7009783
loop_
_publ_author_name
'Cooper, James B.'
'Drew, Michael G. B.'
'Beer, Paul D.'
_publ_section_title
;
 Alkali metal cation cooperative anion recognition by heteroditopic
 bis(calix[4]arene) rhenium(I) bipyridyl and ferrocene receptor
 molecules
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2721
_journal_paper_doi               10.1039/b003569f
_journal_year                    2000
_chemical_formula_sum            'C44 H47 N O14'
_chemical_formula_weight         813.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.322(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.868(17)
_cell_length_b                   14.587(18)
_cell_length_c                   20.29(2)
_cell_measurement_temperature    293(2)
_cell_volume                     4127(8)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 2 min.'
_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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.1000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13134
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.0033(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.2285
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1523P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2219
_refine_ls_wR_factor_ref         0.2906
_reflns_number_gt                2736
_reflns_number_total             7723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003569f.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4126(8)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7009783
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C -0.1684(3) 0.1934(4) 0.1803(2) 0.0681(13) Uani 1 d . . .
C12 C -0.2452(3) 0.2365(3) 0.1905(2) 0.0727(14) Uani 1 d . . .
H12 H -0.2849 0.2749 0.1559 0.087 Uiso 1 calc R . .
C13 C -0.2626(3) 0.2225(3) 0.2520(2) 0.0687(13) Uani 1 d . . .
C14 C -0.2034(3) 0.1673(3) 0.3055(2) 0.0676(13) Uani 1 d . . .
H14 H -0.2161 0.1603 0.3470 0.081 Uiso 1 calc R . .
C15 C -0.1266(3) 0.1233(3) 0.2972(3) 0.0700(13) Uani 1 d . . .
C16 C -0.1112(3) 0.1362(4) 0.2330(3) 0.0693(13) Uani 1 d . . .
C17 C -0.0596(4) 0.0686(4) 0.3572(3) 0.0835(15) Uani 1 d . . .
H17A H -0.0042 0.0499 0.3457 0.100 Uiso 1 calc R . .
H17B H -0.0920 0.0138 0.3642 0.100 Uiso 1 calc R . .
C21 C -0.0267(4) 0.1245(4) 0.4244(3) 0.0756(14) Uani 1 d . . .
C22 C -0.0530(4) 0.1019(4) 0.4823(3) 0.0929(17) Uani 1 d . . .
H22 H -0.0881 0.0488 0.4813 0.111 Uiso 1 calc R . .
C23 C -0.0272(4) 0.1582(5) 0.5412(3) 0.0961(18) Uani 1 d . . .
H23 H -0.0410 0.1407 0.5808 0.115 Uiso 1 calc R . .
C24 C 0.0184(4) 0.2392(5) 0.5406(3) 0.0888(17) Uani 1 d . . .
H24 H 0.0312 0.2783 0.5790 0.107 Uiso 1 calc R . .
C25 C 0.0465(3) 0.2655(4) 0.4847(2) 0.0708(13) Uani 1 d . . .
C26 C 0.0255(3) 0.2044(4) 0.4281(2) 0.0688(13) Uani 1 d . . .
C27 C 0.0811(4) 0.3620(4) 0.4814(2) 0.0773(14) Uani 1 d . . .
H27A H 0.1441 0.3602 0.4772 0.093 Uiso 1 calc R . .
H27B H 0.0867 0.3939 0.5246 0.093 Uiso 1 calc R . .
C31 C 0.0126(4) 0.4138(3) 0.4195(3) 0.0701(13) Uani 1 d . . .
C32 C -0.0838(4) 0.4200(4) 0.4137(3) 0.0803(15) Uani 1 d . . .
H32 H -0.1037 0.3973 0.4492 0.096 Uiso 1 calc R . .
C33 C -0.1496(4) 0.4604(4) 0.3543(3) 0.0912(17) Uani 1 d . . .
H33 H -0.2127 0.4687 0.3518 0.109 Uiso 1 calc R . .
C34 C -0.1227(4) 0.4880(4) 0.2996(3) 0.0872(16) Uani 1 d . . .
H34 H -0.1689 0.5103 0.2589 0.105 Uiso 1 calc R . .
C35 C -0.0274(4) 0.4832(3) 0.3037(2) 0.0726(13) Uani 1 d . . .
C36 C 0.0402(4) 0.4488(3) 0.3660(2) 0.0687(13) Uani 1 d . . .
C37 C 0.0002(4) 0.5075(4) 0.2402(2) 0.0804(15) Uani 1 d . . .
H37A H -0.0035 0.5734 0.2333 0.096 Uiso 1 calc R . .
H37B H 0.0658 0.4886 0.2487 0.096 Uiso 1 calc R . .
C41 C -0.0663(4) 0.4603(4) 0.1744(3) 0.0755(14) Uani 1 d . . .
C42 C -0.1382(4) 0.5095(5) 0.1249(3) 0.0951(18) Uani 1 d . . .
H42 H -0.1410 0.5728 0.1298 0.114 Uiso 1 calc R . .
C43 C -0.2056(5) 0.4669(6) 0.0688(3) 0.108(2) Uani 1 d . . .
H43 H -0.2513 0.5011 0.0346 0.130 Uiso 1 calc R . .
C44 C -0.2043(4) 0.3722(6) 0.0640(3) 0.0993(19) Uani 1 d . . .
H44 H -0.2515 0.3428 0.0273 0.119 Uiso 1 calc R . .
C45 C -0.1341(4) 0.3202(4) 0.1128(2) 0.0748(14) Uani 1 d . . .
C46 C -0.0615(4) 0.3677(4) 0.1646(2) 0.0705(13) Uani 1 d . . .
C47 C -0.1429(4) 0.2168(4) 0.1161(2) 0.0835(16) Uani 1 d . . .
H47A H -0.1924 0.1947 0.0739 0.100 Uiso 1 calc R . .
H47B H -0.0827 0.1880 0.1194 0.100 Uiso 1 calc R . .
O150 O -0.0312(2) 0.0958(3) 0.22488(19) 0.0875(11) Uani 1 d . . .
C151 C -0.0488(4) 0.0138(4) 0.1837(3) 0.0902(16) Uani 1 d . . .
H15A H -0.1091 0.0189 0.1447 0.108 Uiso 1 calc R . .
H15B H -0.0531 -0.0382 0.2123 0.108 Uiso 1 calc R . .
C152 C 0.0303(5) 0.0000(5) 0.1571(3) 0.0943(17) Uani 1 d . . .
O154 O 0.0948(4) 0.0516(4) 0.1633(3) 0.1381(19) Uani 1 d . . .
O153 O 0.0199(3) -0.0784(3) 0.1230(3) 0.1238(16) Uani 1 d . . .
C155 C 0.0943(6) -0.1024(7) 0.0914(6) 0.178(4) Uani 1 d . . .
H15C H 0.1176 -0.0464 0.0770 0.214 Uiso 1 calc R . .
H15D H 0.1481 -0.1317 0.1268 0.214 Uiso 1 calc R . .
C156 C 0.0617(9) -0.1566(12) 0.0373(6) 0.271(8) Uani 1 d . . .
H15E H 0.0342 -0.2102 0.0503 0.326 Uiso 1 calc R . .
H15F H 0.1133 -0.1746 0.0219 0.326 Uiso 1 calc R . .
H15G H 0.0135 -0.1252 -0.0001 0.326 Uiso 1 calc R . .
O250 O 0.0474(2) 0.2267(2) 0.36897(15) 0.0718(9) Uani 1 d . . .
C251 C 0.1450(4) 0.2354(4) 0.3763(3) 0.0792(15) Uani 1 d . . .
H25A H 0.1795 0.2642 0.4211 0.095 Uiso 1 calc R . .
H25B H 0.1503 0.2748 0.3394 0.095 Uiso 1 calc R . .
C252 C 0.1908(5) 0.1432(5) 0.3727(3) 0.0926(18) Uani 1 d . . .
O254 O 0.1640(3) 0.0696(3) 0.3793(2) 0.1159(15) Uani 1 d . . .
O253 O 0.2719(4) 0.1609(4) 0.3613(4) 0.168(3) Uani 1 d . . .
C255 C 0.3273(10) 0.0844(8) 0.3531(9) 0.229(7) Uani 1 d . . .
H25C H 0.2843 0.0344 0.3315 0.275 Uiso 1 calc R . .
H25D H 0.3606 0.1016 0.3214 0.275 Uiso 1 calc R . .
C256 C 0.3934(13) 0.0544(11) 0.4152(8) 0.291(10) Uani 1 d . . .
H25E H 0.4357 0.1038 0.4374 0.349 Uiso 1 calc R . .
H25F H 0.4299 0.0049 0.4059 0.349 Uiso 1 calc R . .
H25G H 0.3607 0.0333 0.4457 0.349 Uiso 1 calc R . .
O350 O 0.1372(2) 0.4466(2) 0.37277(17) 0.0779(10) Uani 1 d . . .
C351 C 0.1798(4) 0.5338(4) 0.3786(3) 0.0849(16) Uani 1 d . . .
H35A H 0.1309 0.5787 0.3554 0.102 Uiso 1 calc R . .
H35B H 0.2265 0.5333 0.3551 0.102 Uiso 1 calc R . .
C352 C 0.2287(4) 0.5613(5) 0.4547(3) 0.0837(16) Uani 1 d . . .
O354 O 0.2557(3) 0.5118(3) 0.5044(2) 0.1169(15) Uani 1 d . . .
O353 O 0.2406(3) 0.6511(3) 0.4575(2) 0.1163(15) Uani 1 d . . .
C355 C 0.2915(6) 0.6920(6) 0.5252(4) 0.140(3) Uani 1 d . . .
H35C H 0.3448 0.6533 0.5518 0.168 Uiso 1 calc R . .
H35D H 0.2489 0.6990 0.5518 0.168 Uiso 1 calc R . .
C356 C 0.3261(8) 0.7802(7) 0.5128(4) 0.172(4) Uani 1 d . . .
H35E H 0.3722 0.7721 0.4899 0.207 Uiso 1 calc R . .
H35F H 0.3557 0.8110 0.5568 0.207 Uiso 1 calc R . .
H35G H 0.2733 0.8162 0.4834 0.207 Uiso 1 calc R . .
N100 N -0.3437(3) 0.2702(4) 0.2616(3) 0.0942(14) Uani 1 d . . .
O101 O -0.3852(4) 0.3297(4) 0.2188(3) 0.139(2) Uani 1 d . . .
O102 O -0.3660(3) 0.2505(3) 0.3122(2) 0.1244(17) Uani 1 d . . .
O450 O 0.0128(2) 0.3182(2) 0.21247(16) 0.0742(9) Uani 1 d . . .
C451 C 0.0773(4) 0.2757(4) 0.1836(3) 0.0851(16) Uani 1 d . . .
H45A H 0.0483 0.2750 0.1328 0.102 Uiso 1 calc R . .
H45B H 0.0876 0.2126 0.1996 0.102 Uiso 1 calc R . .
C452 C 0.1719(5) 0.3237(5) 0.2040(3) 0.0927(17) Uani 1 d . . .
O454 O 0.1972(3) 0.3871(4) 0.2425(3) 0.1183(15) Uani 1 d . . .
O453 O 0.2274(4) 0.2844(5) 0.1756(4) 0.172(3) Uani 1 d . . .
C455 C 0.3201(9) 0.3312(11) 0.1860(8) 0.219(7) Uani 1 d . . .
H45C H 0.3268 0.3458 0.1412 0.263 Uiso 1 calc R . .
H45D H 0.3256 0.3872 0.2129 0.263 Uiso 1 calc R . .
C456 C 0.3759(12) 0.2786(12) 0.2163(12) 0.332(14) Uani 1 d . . .
H45E H 0.3513 0.2179 0.2028 0.398 Uiso 1 calc R . .
H45F H 0.3897 0.2866 0.2658 0.398 Uiso 1 calc R . .
H45G H 0.4335 0.2869 0.2058 0.398 Uiso 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 C11 C16 118.4(5) . . ?
C12 C11 C47 119.5(5) . . ?
C16 C11 C47 121.9(5) . . ?
C13 C12 C11 119.6(5) . . ?
C12 C13 C14 121.8(5) . . ?
C12 C13 N100 118.4(5) . . ?
C14 C13 N100 119.8(5) . . ?
C15 C14 C13 120.1(5) . . ?
C14 C15 C16 117.4(4) . . ?
C14 C15 C17 119.5(5) . . ?
C16 C15 C17 122.9(5) . . ?
O150 C16 C11 119.0(5) . . ?
O150 C16 C15 118.2(5) . . ?
C11 C16 C15 122.6(5) . . ?
C15 C17 C21 111.0(4) . . ?
C26 C21 C22 117.8(5) . . ?
C26 C21 C17 119.9(5) . . ?
C22 C21 C17 122.1(5) . . ?
C23 C22 C21 120.6(6) . . ?
C24 C23 C22 119.6(6) . . ?
C23 C24 C25 122.4(6) . . ?
C24 C25 C26 116.7(5) . . ?
C24 C25 C27 119.7(5) . . ?
C26 C25 C27 122.7(5) . . ?
O250 C26 C21 116.5(4) . . ?
O250 C26 C25 120.5(5) . . ?
C21 C26 C25 122.6(5) . . ?
C25 C27 C31 111.2(4) . . ?
C36 C31 C32 118.9(5) . . ?
C36 C31 C27 122.5(5) . . ?
C32 C31 C27 118.4(5) . . ?
C33 C32 C31 119.4(5) . . ?
C34 C33 C32 120.9(5) . . ?
C33 C34 C35 121.1(5) . . ?
C34 C35 C36 117.8(5) . . ?
C34 C35 C37 120.4(5) . . ?
C36 C35 C37 121.6(5) . . ?
C31 C36 O350 119.3(4) . . ?
C31 C36 C35 121.5(5) . . ?
O350 C36 C35 119.2(5) . . ?
C41 C37 C35 110.6(4) . . ?
C46 C41 C42 118.1(5) . . ?
C46 C41 C37 121.5(5) . . ?
C42 C41 C37 120.3(5) . . ?
C43 C42 C41 121.5(6) . . ?
C42 C43 C44 119.0(6) . . ?
C43 C44 C45 121.3(6) . . ?
C44 C45 C46 117.2(6) . . ?
C44 C45 C47 121.3(5) . . ?
C46 C45 C47 121.0(5) . . ?
C41 C46 O450 118.6(4) . . ?
C41 C46 C45 122.1(5) . . ?
O450 C46 C45 119.0(5) . . ?
C11 C47 C45 108.2(4) . . ?
C16 O150 C151 115.7(4) . . ?
O150 C151 C152 108.7(5) . . ?
O154 C152 O153 123.2(6) . . ?
O154 C152 C151 126.4(6) . . ?
O153 C152 C151 110.4(6) . . ?
C152 O153 C155 117.2(6) . . ?
C156 C155 O153 112.8(8) . . ?
C26 O250 C251 118.1(4) . . ?
O250 C251 C252 112.1(5) . . ?
O254 C252 O253 124.4(6) . . ?
O254 C252 C251 129.1(6) . . ?
O253 C252 C251 106.5(6) . . ?
C252 O253 C255 117.5(7) . . ?
C256 C255 O253 113.5(14) . . ?
C36 O350 C351 113.9(4) . . ?
O350 C351 C352 111.6(4) . . ?
O354 C352 O353 124.3(6) . . ?
O354 C352 C351 127.2(6) . . ?
O353 C352 C351 108.5(5) . . ?
C352 O353 C355 117.9(5) . . ?
O353 C355 C356 107.7(7) . . ?
O102 N100 O101 123.0(5) . . ?
O102 N100 C13 118.7(5) . . ?
O101 N100 C13 118.3(5) . . ?
C46 O450 C451 114.9(4) . . ?
O450 C451 C452 112.6(5) . . ?
O454 C452 O453 122.3(6) . . ?
O454 C452 C451 126.9(6) . . ?
O453 C452 C451 110.7(6) . . ?
C452 O453 C455 115.9(7) . . ?
C456 C455 O453 103.4(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 C12 1.381(7) . ?
C11 C16 1.389(7) . ?
C11 C47 1.517(7) . ?
C12 C13 1.375(7) . ?
C13 C14 1.393(7) . ?
C13 N100 1.463(7) . ?
C14 C15 1.372(6) . ?
C15 C16 1.411(7) . ?
C15 C17 1.507(7) . ?
C16 O150 1.387(6) . ?
C17 C21 1.516(7) . ?
C21 C26 1.388(7) . ?
C21 C22 1.400(8) . ?
C22 C23 1.389(8) . ?
C23 C24 1.364(8) . ?
C24 C25 1.393(7) . ?
C25 C26 1.400(7) . ?
C25 C27 1.509(7) . ?
C26 O250 1.386(6) . ?
C27 C31 1.516(7) . ?
C31 C36 1.385(7) . ?
C31 C32 1.399(7) . ?
C32 C33 1.392(7) . ?
C33 C34 1.363(7) . ?
C34 C35 1.392(7) . ?
C35 C36 1.406(7) . ?
C35 C37 1.524(7) . ?
C36 O350 1.401(6) . ?
C37 C41 1.523(7) . ?
C41 C46 1.372(7) . ?
C41 C42 1.385(7) . ?
C42 C43 1.377(8) . ?
C43 C44 1.385(9) . ?
C44 C45 1.390(8) . ?
C45 C46 1.400(7) . ?
C45 C47 1.517(8) . ?
C46 O450 1.392(6) . ?
O150 C151 1.431(6) . ?
C151 C152 1.469(8) . ?
C152 O154 1.191(7) . ?
C152 O153 1.317(7) . ?
O153 C155 1.501(8) . ?
C155 C156 1.301(12) . ?
O250 C251 1.412(6) . ?
C251 C252 1.521(8) . ?
C252 O254 1.168(7) . ?
C252 O253 1.329(8) . ?
O253 C255 1.431(11) . ?
C255 C256 1.373(17) . ?
O350 C351 1.407(6) . ?
C351 C352 1.514(7) . ?
C352 O354 1.190(6) . ?
C352 O353 1.322(7) . ?
O353 C355 1.446(7) . ?
C355 C356 1.439(11) . ?
N100 O102 1.217(6) . ?
N100 O101 1.232(6) . ?
O450 C451 1.428(6) . ?
C451 C452 1.495(8) . ?
C452 O454 1.186(7) . ?
C452 O453 1.293(7) . ?
O453 C455 1.486(13) . ?
C455 C456 1.141(19) . ?
