#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:30:38 +0100 (lun 21 de mar de 2016) $
#$Revision: 178785 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/39/4103903.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_4103903
loop_
_publ_author_name
'Xiang Lin'
'Irvin Telepeni'
'Alexander J. Blake'
'Anne Dailly'
'Craig M. Brown'
'Jason M. Simmons'
'Marco Zoppi'
'Gavin S. Walker'
'K. Mark Thomas'
'Timothy J. Mays'
'Peter Hubberstey'
'Neil R. Champness'
'Martin Schröder'
_publ_section_title
;
 High Capacity Hydrogen Adsorption in Cu(II) Tetracarboxylate Framework
 Materials: The Role of Pore Size, Ligand Functionalization, and Exposed
 Metal Sites
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2159
_journal_page_last               2171
_journal_paper_doi               10.1021/ja806624j
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C22 H10 Cu2 F4 O10, C3 H7 N O, H2 O'
_chemical_formula_structural
'[Cu2 (C22 O8 H6 F4) (H2 O)2](C3 H7 O N) (H2 O)'
_chemical_formula_sum            'C25 H19 Cu2 F4 N O12'
_chemical_formula_weight         728.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           166
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   18.525(1)
_cell_length_b                   18.525(1)
_cell_length_c                   38.830(2)
_cell_measurement_reflns_used    4649
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.38
_cell_volume                     11540.2(11)
_computing_cell_refinement       'Bruker SAINT version 7.12A (Bruker, 2004)'
_computing_data_collection       'Bruker APEX2 Version 1.0-27 (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ' ? '
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART APEXII CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6907
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_av_sigmaI/netI    0.078
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            54877
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.1603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004/1)'
_exptl_crystal_colour            BLUE
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3293
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.035
_platon_squeeze_details
;
Approximately 61.7% of the unit cell volume comprises a large region of
disordered solvent which could not be modelled as discrete atomic sites. 
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region and thereby produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total count of 323 electrons per unit cell.
The final formula was calculated from the SQUEEZE results combined with
elemental analysis data.
;
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.56
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         3521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0589
_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)+(0.1026P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.164
_refine_ls_wR_factor_ref         0.172
_reflns_number_gt                2772
_reflns_number_total             3521
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja806624j_si_002_5.cif
_cod_data_source_block           NOTT108
_cod_original_cell_volume        11540(2)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4103903
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'x, x-y, z'
'-x+y, y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
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
Cu1 Cu 0.524141(11) 0.475859(11) -0.027656(11) 0.03270(17) Uani 1 2 d S
C1 C 0.36021(17) 0.45132(17) -0.02737(7) 0.0407(6) Uani 1 1 d .
C2 C 0.27968(17) 0.42971(17) -0.04468(7) 0.0412(6) Uani 1 1 d .
C3 C 0.22258(12) 0.4452(2) -0.02784(10) 0.0387(8) Uani 1 2 d S
H3A H 0.2331 0.4661 -0.0050 0.046 Uiso 1 2 calc SR
C4 C 0.26588(18) 0.40113(19) -0.07831(8) 0.0451(6) Uani 1 1 d .
H4A H 0.3054 0.3913 -0.0898 0.054 Uiso 1 1 calc R
C5 C 0.19346(13) 0.3869(3) -0.09515(12) 0.0457(9) Uani 1 2 d S
C6 C 0.17961(15) 0.3592(3) -0.13171(10) 0.0450(9) Uani 1 2 d S
C7 C 0.2377(4) 0.4004(4) -0.15699(17) 0.0515(14) Uani 0.50 1 d P
C8 C 0.1070(4) 0.2899(4) -0.14284(18) 0.0538(14) Uani 0.50 1 d P
O1 O 0.41157(13) 0.44027(15) -0.04426(5) 0.0485(5) Uani 1 1 d .
O2 O 0.37114(12) 0.48172(13) 0.00262(5) 0.0470(5) Uani 1 1 d .
O3 O 0.56116(13) 0.43884(13) -0.07316(12) 0.0896(13) Uani 1 2 d S
F1 F 0.3106(2) 0.4708(3) -0.14846(11) 0.0708(11) Uani 0.50 1 d P
F2 F 0.0465(3) 0.2441(3) -0.11983(10) 0.0724(12) Uani 0.50 1 d P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0441(2) 0.0441(2) 0.0232(2) -0.00085(7) 0.00085(7) 0.0319(2)
C1 0.0466(14) 0.0440(13) 0.0363(14) -0.0001(11) -0.0042(11) 0.0263(12)
C2 0.0443(14) 0.0519(15) 0.0338(13) -0.0023(11) -0.0036(11) 0.0289(12)
C3 0.0399(12) 0.0479(19) 0.0310(18) -0.0024(15) -0.0012(8) 0.0240(10)
C4 0.0473(14) 0.0607(16) 0.0361(14) -0.0054(13) -0.0028(12) 0.0336(13)
C5 0.0457(14) 0.063(2) 0.034(2) -0.0090(17) -0.0045(9) 0.0315(12)
C6 0.0463(13) 0.067(2) 0.0287(19) -0.0082(18) -0.0041(9) 0.0334(12)
C7 0.040(3) 0.067(4) 0.041(3) -0.011(3) 0.003(2) 0.021(3)
C8 0.050(3) 0.068(4) 0.042(3) -0.010(3) 0.004(3) 0.028(3)
O1 0.0508(11) 0.0720(13) 0.0366(11) -0.0108(10) -0.0094(9) 0.0410(10)
O2 0.0476(11) 0.0682(13) 0.0351(11) -0.0102(9) -0.0065(8) 0.0363(10)
O3 0.102(2) 0.102(2) 0.071(3) -0.0279(12) 0.0279(12) 0.055(3)
F1 0.052(2) 0.082(3) 0.050(2) -0.014(2) 0.0006(18) 0.0132(19)
F2 0.061(2) 0.086(3) 0.038(2) -0.0118(19) 0.0099(18) 0.013(2)
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'
Cu Cu 0.3201 1.2651 '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'
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
O2 Cu1 O2 88.67(13) 19_665 4
O2 Cu1 O1 168.14(8) 19_665 .
O2 Cu1 O1 89.87(10) 4 .
O1 Cu1 O1 89.13(14) 22_665 .
O2 Cu1 O3 97.37(11) 19_665 .
O1 Cu1 O3 94.49(12) . .
O1 C1 C2 117.2(2) . .
O2 C1 C2 116.7(2) . .
C4 C2 C3 120.6(3) . .
C4 C2 C1 119.7(2) . .
C3 C2 C1 119.5(3) . .
C2 C3 C2 119.5(4) . 24
C2 C3 H3A 120.2 . .
C2 C3 H3A 120.2 24 .
C2 C4 C5 119.4(3) . .
C2 C4 H4A 120.3 . .
C5 C4 H4A 120.3 . .
C4 C5 C4 120.4(4) . 24
C4 C5 C6 119.78(19) . .
C4 C5 C6 119.78(19) 24 .
C7 C6 C5 122.6(4) . .
C8 C6 C5 122.5(4) 24 .
C8 C7 F1 117.4(6) 31_554 .
C8 C7 C6 123.8(6) 31_554 .
F1 C7 C6 118.8(5) . .
F1 C7 C7 120.6(3) . 24
F2 C8 C7 119.1(6) . 31_554
F2 C8 C6 119.5(5) . .
C7 C8 C6 121.4(6) 31_554 .
F2 C8 C8 121.1(4) . 24
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9552(19) .
Cu1 O2 1.950(2) 4
Cu1 O3 2.130(3) .
C1 O1 1.254(3) .
C1 O2 1.266(3) .
C1 C2 1.497(4) .
C2 C4 1.385(4) .
C2 C3 1.390(3) .
C4 C5 1.394(3) .
C5 C6 1.488(6) .
C6 C7 1.372(7) .
C6 C8 1.385(7) .
C7 C8 1.356(9) 31_554
C7 F1 1.368(7) .
C7 C7 1.390(12) 24
C8 F2 1.351(7) .
C8 C8 1.404(14) 24
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.072 -0.054 -0.002 7128.2 322.8
