#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:26:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179110 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/72/4307267.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_4307267
loop_
_publ_author_name
'S. Skanthakumar'
'Mark R. Antonio'
'Richard E. Wilson'
'L. Soderholm'
_publ_contact_author_address
;Chemistry Division
Argonne National Laboratory
9700 South Cass Avenue
Argonne, IL 60439
;
_publ_contact_author_email       ls@anl.gov
_publ_contact_author_name        'L. Soderholm'
_publ_contact_author_phone       630-252-4364
_publ_section_title
;
The Curium Aqua Ion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3485
_journal_page_last               3491
_journal_paper_doi               10.1021/ic061798b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '3(C F3 O3 S), 9(H2 O), Cm'
_chemical_formula_sum            'C3 H18 Cm F9 O18 S3'
_chemical_formula_weight         857.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.860(2)
_cell_length_b                   13.860(2)
_cell_length_c                   7.3300(15)
_cell_measurement_reflns_used    19586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.87
_cell_measurement_theta_min      4.05
_cell_volume                     1219.4(4)
_computing_cell_refinement       'APEX II, SAINT+ (Bruker, 2004)'
_computing_data_collection       'APEX II (Bruker, 2004)'
_computing_data_reduction        'SAINT+ (Bruker, 2004)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega scans'
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0124
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19586
_diffrn_reflns_theta_full        32.87
_diffrn_reflns_theta_max         32.87
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    3.738
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_correction_T_min  0.3800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.544
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0115
_refine_ls_R_factor_gt           0.0112
_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/[σ²(Fo²)+(0.0100P)²+0.9033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0286
_refine_ls_wR_factor_ref         0.0286
_reflns_number_gt                1544
_reflns_number_total             1570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061798bsi20061221_123844.cif
_cod_data_source_block           proton
_cod_database_code               4307267
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cm1 Cm 0.6667 0.3333 0.2500 0.00929(3) Uani 1 6 d S . .
S1 S 0.37856(4) 0.32025(4) 0.7500 0.01278(8) Uani 1 2 d S . .
O1 O 0.79197(8) 0.33690(8) 0.48957(14) 0.01508(17) Uani 1 1 d . . .
O2 O 0.65199(13) 0.14280(12) 0.2500 0.0162(2) Uani 1 2 d S . .
O3 O 0.39893(9) 0.38368(9) 0.58282(14) 0.01904(19) Uani 1 1 d . . .
F1 F 0.17514(11) 0.28271(13) 0.7500 0.0301(3) Uani 1 2 d S . .
O4 O 0.42482(12) 0.24675(12) 0.7500 0.0171(3) Uani 1 2 d S . .
F2 F 0.19816(9) 0.16096(9) 0.60253(18) 0.0390(3) Uani 1 1 d . . .
C1 C 0.22808(17) 0.22492(18) 0.7500 0.0223(4) Uani 1 2 d S . .
H1 H 0.8552(19) 0.3595(19) 0.472(3) 0.030(6) Uiso 1 1 d . . .
H3 H 0.6458(19) 0.1041(19) 0.336(3) 0.034(6) Uiso 1 1 d . . .
H2 H 0.773(2) 0.285(2) 0.558(4) 0.037(6) Uiso 1 1 d . . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cm Cm -7.3248 4.6989 '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
O1 Cm1 O1 139.136(19) . 12_666 ?
O1 Cm1 O1 91.44(5) . 10_556 ?
O1 Cm1 O1 74.41(4) 12_666 10_556 ?
O1 Cm1 O1 74.41(4) . 3_665 ?
O1 Cm1 O1 91.44(5) 12_666 3_665 ?
O1 Cm1 O1 139.136(19) 10_556 3_665 ?
O1 Cm1 O1 74.41(4) . 2_655 ?
O1 Cm1 O1 139.136(19) 12_666 2_655 ?
O1 Cm1 O1 139.136(19) 10_556 2_655 ?
O1 Cm1 O1 74.41(4) 3_665 2_655 ?
O1 Cm1 O1 139.136(19) . 11_656 ?
O1 Cm1 O1 74.41(4) 12_666 11_656 ?
O1 Cm1 O1 74.41(4) 10_556 11_656 ?
O1 Cm1 O1 139.136(19) 3_665 11_656 ?
O1 Cm1 O1 91.44(5) 2_655 11_656 ?
O1 Cm1 O2 73.11(3) . . ?
O1 Cm1 O2 66.14(3) 12_666 . ?
O1 Cm1 O2 73.11(3) 10_556 . ?
O1 Cm1 O2 66.14(3) 3_665 . ?
O1 Cm1 O2 134.03(3) 2_655 . ?
O1 Cm1 O2 134.03(3) 11_656 . ?
O1 Cm1 O2 66.14(3) . 2_655 ?
O1 Cm1 O2 134.03(3) 12_666 2_655 ?
O1 Cm1 O2 66.14(3) 10_556 2_655 ?
O1 Cm1 O2 134.03(3) 3_665 2_655 ?
O1 Cm1 O2 73.11(3) 2_655 2_655 ?
O1 Cm1 O2 73.11(3) 11_656 2_655 ?
O2 Cm1 O2 120.0 . 2_655 ?
O1 Cm1 O2 134.03(3) . 3_665 ?
O1 Cm1 O2 73.11(3) 12_666 3_665 ?
O1 Cm1 O2 134.03(3) 10_556 3_665 ?
O1 Cm1 O2 73.11(3) 3_665 3_665 ?
O1 Cm1 O2 66.14(3) 2_655 3_665 ?
O1 Cm1 O2 66.14(3) 11_656 3_665 ?
O2 Cm1 O2 120.0 . 3_665 ?
O2 Cm1 O2 120.0 2_655 3_665 ?
O1 Cm1 H1 12.9(5) . . ?
O1 Cm1 H1 137.5(4) 12_666 . ?
O1 Cm1 H1 79.5(5) 10_556 . ?
O1 Cm1 H1 86.9(5) 3_665 . ?
O1 Cm1 H1 80.8(5) 2_655 . ?
O1 Cm1 H1 129.3(5) 11_656 . ?
O2 Cm1 H1 74.5(4) . . ?
O2 Cm1 H1 56.6(5) 2_655 . ?
O2 Cm1 H1 144.7(5) 3_665 . ?
O1 Cm1 H3 65.1(4) . . ?
O1 Cm1 H3 75.0(4) 12_666 . ?
O1 Cm1 H3 82.5(4) 10_556 . ?
O1 Cm1 H3 56.7(4) 3_665 . ?
O1 Cm1 H3 122.3(4) 2_655 . ?
O1 Cm1 H3 145.6(4) 11_656 . ?
O2 Cm1 H3 11.7(4) . . ?
O2 Cm1 H3 120.0(4) 2_655 . ?
O2 Cm1 H3 118.6(4) 3_665 . ?
H1 Cm1 H3 68.7(6) . . ?
O1 Cm1 H2 13.6(5) . . ?
O1 Cm1 H2 129.2(5) 12_666 . ?
O1 Cm1 H2 97.2(5) 10_556 . ?
O1 Cm1 H2 62.3(5) 3_665 . ?
O1 Cm1 H2 78.0(5) 2_655 . ?
O1 Cm1 H2 152.7(5) 11_656 . ?
O2 Cm1 H2 63.5(5) . . ?
O2 Cm1 H2 79.7(5) 2_655 . ?
O2 Cm1 H2 128.6(5) 3_665 . ?
H1 Cm1 H2 24.8(6) . . ?
H3 Cm1 H2 54.2(6) . . ?
O4 S1 O3 113.90(5) . 10_557 ?
O4 S1 O3 113.90(5) . . ?
O3 S1 O3 115.22(9) 10_557 . ?
O4 S1 C1 103.75(9) . . ?
O3 S1 C1 104.12(6) 10_557 . ?
O3 S1 C1 104.12(6) . . ?
Cm1 O1 H1 122.3(18) . . ?
Cm1 O1 H2 120.8(18) . . ?
H1 O1 H2 105(2) . . ?
Cm1 O2 H3 128.2(16) . . ?
F2 C1 F2 109.20(19) . 10_557 ?
F2 C1 F1 108.69(12) . . ?
F2 C1 F1 108.69(12) 10_557 . ?
F2 C1 S1 110.22(11) . . ?
F2 C1 S1 110.22(11) 10_557 . ?
F1 C1 S1 109.79(15) . . ?
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
Cm1 O1 2.4528(10) . ?
Cm1 O1 2.4528(10) 12_666 ?
Cm1 O1 2.4528(10) 10_556 ?
Cm1 O1 2.4528(10) 3_665 ?
Cm1 O1 2.4528(10) 2_655 ?
Cm1 O1 2.4528(10) 11_656 ?
Cm1 O2 2.5452(14) . ?
Cm1 O2 2.5452(14) 2_655 ?
Cm1 O2 2.5452(14) 3_665 ?
Cm1 H1 2.94(2) . ?
Cm1 H3 3.11(2) . ?
Cm1 H2 2.95(3) . ?
S1 O4 1.4499(14) . ?
S1 O3 1.4512(10) 10_557 ?
S1 O3 1.4512(10) . ?
S1 C1 1.828(2) . ?
O1 H1 0.78(2) . ?
O1 H2 0.81(3) . ?
O2 H3 0.80(2) . ?
F1 C1 1.330(2) . ?
F2 C1 1.3262(16) . ?
C1 F2 1.3262(16) 10_557 ?
