#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:24:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179842 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/38/7013893.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_7013893
loop_
_publ_author_name
'Starynowicz, Przemysław'
_publ_section_title
;
 Two complexes of Sm(II) with crown ethers-electrochemical synthesis,
 structure and spectroscopy.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              825
_journal_page_last               832
_journal_paper_doi               10.1039/b316253b
_journal_year                    2004
_chemical_formula_sum            'C20 H40 Cl2 O18 Sm'
_chemical_formula_weight         789.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           161
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'P 3* -2n'
_symmetry_space_group_name_H-M   'R 3 c :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.30(6)
_cell_angle_beta                 108.30(6)
_cell_angle_gamma                108.30(6)
_cell_formula_units_Z            6
_cell_length_a                   18.053(11)
_cell_length_b                   18.053(11)
_cell_length_c                   18.053(11)
_cell_measurement_reflns_used    2931
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3.5
_cell_volume                     4715(7)
_computing_cell_refinement       'Kuma KM4 software (1999)'
_computing_data_collection       'Kuma KM4 software (1999)'
_computing_data_reduction        'Kuma KM4 software (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      240(2)
_diffrn_measured_fraction_theta_full 0.674
_diffrn_measured_fraction_theta_max 0.674
_diffrn_measurement_device_type  'Kuma KM4 with a CCD counter'
_diffrn_measurement_method       'ω scan'
_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  0.0981
_diffrn_reflns_av_sigmaI/netI    0.2135
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16128
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    2.112
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   'analytical, from the crystal shape'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat needle'
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.839
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         3499
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.839
_refine_ls_R_factor_all          0.1464
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                2079
_reflns_number_total             3499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b316253b.txt
_cod_data_source_block           test
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^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^)+(0.0000P)^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        4715(5)
_cod_original_sg_symbol_H-M      R3c
_cod_database_code               7013893
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, y+1/2'
'z+1/2, y+1/2, x+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
Sm Sm 0.03844(8) 0.89348(7) 0.29023(7) 0.04029(19) Uani 1 d . . .
Cl1 Cl -0.0221(3) 1.1748(3) 0.6684(3) 0.0663(13) Uani 1 d . . .
Cl2 Cl 0.3802(4) 1.0835(4) 0.2839(4) 0.0876(17) Uani 1 d . . .
O1 O 0.0306(7) 0.8717(9) 0.4310(7) 0.068(4) Uani 1 d . . .
O2 O -0.0468(8) 0.7287(7) 0.2729(9) 0.064(3) Uani 1 d . . .
O3 O -0.1308(7) 0.7848(9) 0.1656(6) 0.075(4) Uani 1 d . . .
O4 O -0.0612(9) 0.9669(10) 0.2263(11) 0.092(4) Uani 1 d . . .
O5 O -0.0265(8) 0.9775(8) 0.3846(9) 0.076(4) Uani 1 d . . .
O11 O 0.0328(10) 0.8851(12) 0.1334(9) 0.089(5) Uani 1 d . . .
O12 O 0.1461(8) 1.0325(8) 0.2873(10) 0.087(4) Uani 1 d . . .
O13 O 0.1811(8) 1.0273(9) 0.4384(9) 0.079(4) Uani 1 d . . .
O14 O 0.1832(7) 0.8715(9) 0.3613(9) 0.072(3) Uani 1 d . . .
O15 O 0.0639(8) 0.7662(8) 0.1876(8) 0.084(4) Uani 1 d . . .
O21A O -0.0864(17) 1.2048(16) 0.6780(14) 0.080(7) Uiso 0.50 d P . .
O21B O -0.0268(15) 1.2562(14) 0.7058(14) 0.062(6) Uiso 0.50 d P . .
O22 O -0.0566(9) 1.1034(8) 0.6847(8) 0.107(4) Uani 1 d . . .
O23A O -0.0186(19) 1.1609(15) 0.5933(18) 0.076(8) Uiso 0.50 d P . .
O23B O -0.0691(18) 1.1426(15) 0.5730(16) 0.078(9) Uiso 0.50 d P . .
O24A O 0.0655(13) 1.2278(12) 0.7395(13) 0.057(6) Uiso 0.50 d P . .
O24B O 0.0635(18) 1.1841(17) 0.675(2) 0.120(9) Uiso 0.50 d P . .
O31 O 0.3266(12) 1.1082(14) 0.2419(14) 0.207(10) Uani 1 d . . .
O32 O 0.4019(9) 1.1091(10) 0.3708(10) 0.143(6) Uani 1 d . . .
O33 O 0.4546(9) 1.0998(10) 0.2726(9) 0.134(6) Uani 1 d . . .
O34 O 0.3262(11) 0.9879(17) 0.2491(12) 0.200(8) Uani 1 d . . .
C1 C 0.0151(13) 0.7840(14) 0.4234(12) 0.085(7) Uani 1 d . . .
H1A H 0.0050 0.7785 0.4715 0.102 Uiso 1 calc R . .
H1B H 0.0660 0.7753 0.4259 0.102 Uiso 1 calc R . .
C2 C -0.0623(10) 0.7179(10) 0.3390(13) 0.073(6) Uani 1 d . . .
H2A H -0.0730 0.6593 0.3319 0.088 Uiso 1 calc R . .
H2B H -0.1138 0.7250 0.3375 0.088 Uiso 1 calc R . .
C3 C -0.1186(16) 0.6711(12) 0.1879(15) 0.101(9) Uani 1 d . . .
H3A H -0.1494 0.6151 0.1858 0.121 Uiso 1 calc R . .
H3B H -0.0965 0.6608 0.1451 0.121 Uiso 1 calc R . .
C4 C -0.1792(12) 0.7062(14) 0.1649(12) 0.077(7) Uani 1 d . . .
H4A H -0.2282 0.6654 0.1072 0.092 Uiso 1 calc R . .
H4B H -0.2016 0.7176 0.2073 0.092 Uiso 1 calc R . .
C5 C -0.1872(12) 0.8181(18) 0.1305(15) 0.118(10) Uani 1 d . . .
H5A H -0.2216 0.8247 0.1616 0.142 Uiso 1 calc R . .
H5B H -0.2269 0.7783 0.0689 0.142 Uiso 1 calc R . .
C6 C -0.1292(14) 0.9065(19) 0.1416(14) 0.124(10) Uani 1 d . . .
H6A H -0.1034 0.8966 0.1020 0.149 Uiso 1 calc R . .
H6B H -0.1662 0.9329 0.1234 0.149 Uiso 1 calc R . .
C8 C -0.0297(14) 1.0460(15) 0.3722(18) 0.111(9) Uani 1 d . . .
H8A H 0.0288 1.0876 0.3879 0.133 Uiso 1 calc R . .
H8B H -0.0502 1.0752 0.4102 0.133 Uiso 1 calc R . .
C7 C -0.0862(18) 1.0191(19) 0.284(2) 0.111(9) Uani 1 d . . .
H7A H -0.0824 1.0701 0.2751 0.133 Uiso 1 calc R . .
H7B H -0.1463 0.9845 0.2706 0.133 Uiso 1 calc R . .
C9 C 0.0037(11) 0.9963(14) 0.4738(15) 0.087(7) Uani 1 d . . .
H9A H -0.0305 1.0183 0.4978 0.104 Uiso 1 calc R . .
H9B H 0.0649 1.0396 0.5081 0.104 Uiso 1 calc R . .
C10 C -0.0083(13) 0.9095(16) 0.4744(12) 0.102(8) Uani 1 d . . .
H10A H 0.0171 0.9191 0.5346 0.123 Uiso 1 calc R . .
H10B H -0.0704 0.8698 0.4467 0.123 Uiso 1 calc R . .
C11 C 0.0979(14) 0.962(2) 0.1404(16) 0.137(12) Uani 1 d . . .
H11A H 0.0744 0.9668 0.0869 0.165 Uiso 1 calc R . .
H11B H 0.1491 0.9532 0.1445 0.165 Uiso 1 calc R . .
C12 C 0.1260(14) 1.0457(15) 0.2161(18) 0.115(10) Uani 1 d . . .
H12A H 0.1768 1.0921 0.2228 0.138 Uiso 1 calc R . .
H12B H 0.0791 1.0624 0.2075 0.138 Uiso 1 calc R . .
C13 C 0.1999(12) 1.1113(11) 0.3686(16) 0.090(8) Uani 1 d . . .
H13A H 0.2432 1.1537 0.3625 0.108 Uiso 1 calc R . .
H13B H 0.1640 1.1368 0.3850 0.108 Uiso 1 calc R . .
C14 C 0.2425(16) 1.0905(17) 0.4345(16) 0.119(9) Uani 1 d . . .
H14A H 0.2823 1.0699 0.4206 0.143 Uiso 1 calc R . .
H14B H 0.2764 1.1425 0.4910 0.143 Uiso 1 calc R . .
C15 C 0.2292(16) 0.9915(17) 0.4888(13) 0.113(9) Uani 1 d . . .
H15A H 0.2798 1.0400 0.5419 0.135 Uiso 1 calc R . .
H15B H 0.1911 0.9573 0.5061 0.135 Uiso 1 calc R . .
C16 C 0.2583(12) 0.9375(15) 0.4408(14) 0.085(7) Uani 1 d . . .
H16A H 0.3020 0.9722 0.4289 0.102 Uiso 1 calc R . .
H16B H 0.2840 0.9114 0.4741 0.102 Uiso 1 calc R . .
C17 C 0.2051(13) 0.8174(14) 0.3039(18) 0.111(9) Uani 1 d . . .
H17A H 0.2441 0.7992 0.3356 0.133 Uiso 1 calc R . .
H17B H 0.2338 0.8488 0.2781 0.133 Uiso 1 calc R . .
C18 C 0.1218(19) 0.7413(16) 0.2360(19) 0.125(11) Uani 1 d . . .
H18A H 0.1330 0.7010 0.1963 0.150 Uiso 1 calc R . .
H18B H 0.0941 0.7110 0.2632 0.150 Uiso 1 calc R . .
C19 C 0.0635(18) 0.7674(16) 0.1037(16) 0.118(10) Uani 1 d . . .
H19A H 0.1231 0.7991 0.1142 0.142 Uiso 1 calc R . .
H19B H 0.0390 0.7077 0.0586 0.142 Uiso 1 calc R . .
C20 C 0.0144(16) 0.807(2) 0.0752(17) 0.122(10) Uani 1 d . . .
H20A H 0.0213 0.8127 0.0258 0.146 Uiso 1 calc R . .
H20B H -0.0469 0.7677 0.0535 0.146 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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
O12 Sm O5 97.4(4) . . no
O12 Sm O13 58.7(5) . . no
O5 Sm O13 74.9(4) . . no
O12 Sm O3 124.1(4) . . no
O5 Sm O3 86.6(4) . . no
O13 Sm O3 161.5(4) . . no
O12 Sm O4 73.3(4) . . no
O5 Sm O4 58.4(5) . . no
O13 Sm O4 105.8(5) . . no
O3 Sm O4 61.9(5) . . no
O12 Sm O14 86.6(4) . . no
O5 Sm O14 124.5(4) . . no
O13 Sm O14 60.3(4) . . no
O3 Sm O14 135.1(5) . . no
O4 Sm O14 159.8(4) . . no
O12 Sm O15 99.3(4) . . no
O5 Sm O15 162.9(4) . . no
O13 Sm O15 117.1(4) . . no
O3 Sm O15 81.2(4) . . no
O4 Sm O15 123.9(5) . . no
O14 Sm O15 60.2(4) . . no
O12 Sm O1 129.1(4) . . no
O5 Sm O1 58.8(4) . . no
O13 Sm O1 71.2(4) . . no
O3 Sm O1 100.5(3) . . no
O4 Sm O1 115.2(4) . . no
O14 Sm O1 76.1(4) . . no
O15 Sm O1 111.7(4) . . no
O12 Sm O2 163.4(4) . . no
O5 Sm O2 98.9(4) . . no
O13 Sm O2 123.7(5) . . no
O3 Sm O2 59.8(4) . . no
O4 Sm O2 118.1(4) . . no
O14 Sm O2 82.0(4) . . no
O15 Sm O2 64.6(4) . . no
O1 Sm O2 59.4(4) . . no
O12 Sm O11 59.9(5) . . no
O5 Sm O11 127.1(5) . . no
O13 Sm O11 116.7(5) . . no
O3 Sm O11 73.5(4) . . no
O4 Sm O11 69.1(5) . . no
O14 Sm O11 102.6(4) . . no
O15 Sm O11 60.4(5) . . no
O1 Sm O11 170.3(5) . . no
O2 Sm O11 111.0(5) . . no
O23A Cl1 O22 120.0(12) . . no
O23A Cl1 O24A 109.0(15) . . no
O22 Cl1 O24A 103.6(9) . . no
O23A Cl1 O21B 111.3(13) . . no
O22 Cl1 O21B 122.8(11) . . no
O24A Cl1 O21B 80.7(12) . . no
O23A Cl1 O21A 114.5(15) . . no
O22 Cl1 O21A 93.4(12) . . no
O24A Cl1 O21A 115.5(13) . . no
O21B Cl1 O21A 40.4(10) . . no
O23A Cl1 O23B 31.6(12) . . no
O22 Cl1 O23B 106.5(11) . . no
O24A Cl1 O23B 139.8(13) . . no
O21B Cl1 O23B 104.0(13) . . no
O21A Cl1 O23B 88.8(14) . . no
O23A Cl1 O24B 67.5(15) . . no
O22 Cl1 O24B 106.0(13) . . no
O24A Cl1 O24B 47.2(11) . . no
O21B Cl1 O24B 115.9(15) . . no
O21A Cl1 O24B 156.2(15) . . no
O23B Cl1 O24B 98.4(16) . . no
O31 Cl2 O32 117.0(11) . . no
O31 Cl2 O33 114.6(10) . . no
O32 Cl2 O33 109.9(9) . . no
O31 Cl2 O34 104.4(12) . . no
O32 Cl2 O34 98.9(10) . . no
O33 Cl2 O34 110.6(11) . . no
C10 O1 C1 114.1(15) . . no
C10 O1 Sm 120.6(12) . . no
C1 O1 Sm 114.6(9) . . no
C2 O2 C3 114.0(14) . . no
C2 O2 Sm 121.0(10) . . no
C3 O2 Sm 111.8(11) . . no
C5 O3 C4 110.6(16) . . no
C5 O3 Sm 121.4(13) . . no
C4 O3 Sm 120.5(11) . . no
C6 O4 C7 115.1(18) . . no
C6 O4 Sm 110.6(13) . . no
C7 O4 Sm 118.6(12) . . no
C8 O5 C9 112.1(17) . . no
C8 O5 Sm 113.4(13) . . no
C9 O5 Sm 118.7(11) . . no
C20 O11 C11 118.0(19) . . no
C20 O11 Sm 114.7(15) . . no
C11 O11 Sm 115.2(12) . . no
C12 O12 C13 114.3(18) . . no
C12 O12 Sm 121.9(12) . . no
C13 O12 Sm 116.9(12) . . no
C14 O13 C15 106.2(19) . . no
C14 O13 Sm 120.8(14) . . no
C15 O13 Sm 109.7(11) . . no
C16 O14 C17 112.0(15) . . no
C16 O14 Sm 122.3(11) . . no
C17 O14 Sm 119.0(12) . . no
C18 O15 C19 119.7(16) . . no
C18 O15 Sm 113.7(12) . . no
C19 O15 Sm 116.9(12) . . no
O21B O21A Cl1 69(2) . . no
O21A O21B Cl1 70(2) . . no
O23B O23A Cl1 85(3) . . no
O23B O23A O24B 143(4) . . no
Cl1 O23A O24B 60.5(16) . . no
O23A O23B Cl1 64(3) . . no
O24B O24A Cl1 67.4(17) . . no
O24A O24B Cl1 65.4(18) . . no
O24A O24B O23A 111(3) . . no
Cl1 O24B O23A 52.1(13) . . no
O1 C1 C2 108.6(13) . . no
O2 C2 C1 108.5(14) . . no
O2 C3 C4 111.9(15) . . no
O3 C4 C3 105.8(16) . . no
O3 C5 C6 107.1(15) . . no
O4 C6 C5 116.3(18) . . no
O5 C8 C7 111(2) . . no
C8 C7 O4 109.5(18) . . no
O5 C9 C10 105.1(16) . . no
O1 C10 C9 111.8(17) . . no
O11 C11 C12 115.1(19) . . no
O12 C12 C11 107(2) . . no
C14 C13 O12 108.7(18) . . no
O13 C14 C13 109(2) . . no
C16 C15 O13 113.7(17) . . no
O14 C16 C15 106.6(16) . . no
O14 C17 C18 105.7(18) . . no
O15 C18 C17 111.7(19) . . no
C20 C19 O15 110(2) . . no
O11 C20 C19 117(3) . . no
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
Sm O12 2.677(12) . yes
Sm O5 2.706(12) . yes
Sm O13 2.708(15) . yes
Sm O3 2.719(13) . yes
Sm O4 2.735(12) . yes
Sm O14 2.739(11) . yes
Sm O15 2.730(11) . yes
Sm O1 2.730(11) . yes
Sm O2 2.748(11) . yes
Sm O11 2.755(13) . yes
Cl1 O23A 1.32(2) . no
Cl1 O22 1.409(11) . no
Cl1 O24A 1.438(19) . no
Cl1 O21B 1.45(2) . no
Cl1 O21A 1.46(2) . no
Cl1 O23B 1.47(2) . no
Cl1 O24B 1.46(3) . no
Cl2 O31 1.316(14) . no
Cl2 O32 1.368(14) . no
Cl2 O33 1.378(13) . no
Cl2 O34 1.48(2) . no
O1 C10 1.372(19) . no
O1 C1 1.469(19) . no
O2 C2 1.365(18) . no
O2 C3 1.42(2) . no
O3 C5 1.42(2) . no
O3 C4 1.41(2) . no
O4 C6 1.40(2) . no
O4 C7 1.46(2) . no
O5 C8 1.34(2) . no
O5 C9 1.41(2) . no
O11 C20 1.33(3) . no
O11 C11 1.45(2) . no
O12 C12 1.34(2) . no
O12 C13 1.430(19) . no
O13 C14 1.36(2) . no
O13 C15 1.49(3) . no
O14 C16 1.42(2) . no
O14 C17 1.43(2) . no
O15 C18 1.42(2) . no
O15 C19 1.52(2) . no
O21A O21B 1.01(2) . no
O23A O23B 0.77(3) . no
O23A O24B 1.55(3) . no
O24A O24B 1.16(3) . no
C1 C2 1.47(2) . no
C3 C4 1.45(2) . no
C5 C6 1.52(3) . no
C8 C7 1.41(3) . no
C9 C10 1.52(2) . no
C11 C12 1.48(3) . no
C13 C14 1.43(3) . no
C15 C16 1.43(2) . no
C17 C18 1.46(3) . no
C19 C20 1.38(3) . no
