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#$Date: 2016-03-22 11:16:28 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178892 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/21/4112174.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_4112174
loop_
_publ_author_name
'Long Pan'
'Michelle B. Sander'
'Xiaoying Huang'
'Jing Li'
'Milton Smith'
'Edward Bittner'
'Bradley Bockrath'
'J. Karl Johnson'
_publ_contact_author             'Li Jing'
_publ_contact_author_address
; Department of Chemistry and Chemical Biology,
Rutgers University,
Piscataway, NJ 08854, USA
;
_publ_contact_author_email       jingli@rutchem.rutgers.edu
_publ_contact_author_fax         +1(732)445-5312
_publ_contact_author_phone       +1(732)445-2774
_publ_section_title
;
 Microporous Metal Organic Materials: Promising Candidates as Sorbents for
 Hydrogen Storage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1308
_journal_page_last               1309
_journal_paper_doi               10.1021/ja0392871
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         Cu(hfipbb)(H2hfipbb)0.5
_chemical_formula_sum            'C51 H26 Cu2 F18 O12'
_chemical_formula_weight         1299.80
_chemical_name_systematic
; 
catena-(mu4-4,4'(hexafluoroisopropylidene)bis(benzenecarboxylato)
-half(mu2-4,4'(hexafluoroisopropylidene)bis(benzoic acid)copper(II) 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 107.02(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.723(4)
_cell_length_b                   7.2710(10)
_cell_length_c                   20.481(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.95
_cell_measurement_theta_min      7.63
_cell_volume                     2666.1(10)
_computing_cell_refinement       CAD4/PC
_computing_data_collection       CAD4/PC
_computing_data_reduction        XCAD4/PC
_computing_molecular_graphics    'Material Studio'
_computing_publication_material  'Windows Word2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 '
_diffrn_measurement_method       ω
_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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10702
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        +-5.0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            light-blue
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                3397
_reflns_number_total             5214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0392871si20031028_031215.cif
_cod_data_source_block           Compound_MS2-10B1
_cod_original_cell_volume        2666.1(9)
_cod_database_code               4112174
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
Cu Cu 0.52790(2) 0.14651(6) 0.47800(2) 0.02932(12) Uani 1 1 d .
F1 F 0.02389(13) 0.2530(3) 0.33169(12) 0.0599(7) Uani 1 1 d .
F2 F -0.04635(11) 0.4760(4) 0.34069(12) 0.0667(8) Uani 1 1 d .
F3 F 0.01035(12) 0.3182(4) 0.42902(12) 0.0657(8) Uani 1 1 d .
F4 F 0.13119(13) 0.7943(3) 0.44902(11) 0.0585(7) Uani 1 1 d .
F5 F 0.01544(13) 0.7336(4) 0.43405(11) 0.0642(8) Uani 1 1 d .
F6 F 0.09998(13) 0.5709(4) 0.50260(10) 0.0650(8) Uani 1 1 d .
F7 F 0.70913(16) 1.0412(4) 0.15483(15) 0.0896(10) Uani 1 1 d .
F8 F 0.66830(15) 1.1026(3) 0.23960(16) 0.0875(10) Uani 1 1 d .
F9 F 0.62606(13) 0.8698(4) 0.17600(13) 0.0702(8) Uani 1 1 d .
O1 O 0.42911(13) 0.2586(3) 0.45819(13) 0.0408(7) Uani 1 1 d .
O2 O 0.38165(13) 0.0144(4) 0.49615(12) 0.0405(7) Uani 1 1 d .
O3 O 0.05402(14) 0.7708(4) 0.07204(12) 0.0427(7) Uani 1 1 d .
O4 O 0.00473(14) 1.0174(4) 0.10838(12) 0.0439(7) Uani 1 1 d .
O5 O 0.58746(12) 0.3557(4) 0.43569(12) 0.0388(6) Uani 1 1 d .
O6 O 0.69066(16) 0.1965(4) 0.44201(16) 0.0752(11) Uani 1 1 d .
H1 H 0.6605 0.0983 0.4680 0.090 Uiso 1 1 d R
C1 C 0.3763(2) 0.1745(5) 0.46984(17) 0.0331(9) Uani 1 1 d .
C2 C 0.30111(19) 0.2650(5) 0.45015(17) 0.0338(9) Uani 1 1 d .
C3 C 0.29309(19) 0.4382(5) 0.42286(17) 0.0342(9) Uani 1 1 d .
H2 H 0.3347 0.5017 0.4187 0.041 Uiso 1 1 calc R
C4 C 0.22378(19) 0.5185(5) 0.40163(18) 0.0383(10) Uani 1 1 d .
H3 H 0.2187 0.6358 0.3827 0.046 Uiso 1 1 calc R
C5 C 0.16140(19) 0.4275(5) 0.40810(17) 0.0315(9) Uani 1 1 d .
C6 C 0.1706(2) 0.2554(6) 0.4377(2) 0.0524(12) Uani 1 1 d .
H4 H 0.1297 0.1941 0.4443 0.063 Uiso 1 1 calc R
C7 C 0.2398(2) 0.1738(6) 0.4577(2) 0.0512(12) Uani 1 1 d .
H5 H 0.2451 0.0562 0.4763 0.061 Uiso 1 1 calc R
C8 C 0.08460(19) 0.5247(5) 0.38396(17) 0.0333(9) Uani 1 1 d .
C9 C 0.07553(18) 0.6259(5) 0.31613(17) 0.0310(9) Uani 1 1 d .
C10 C 0.0903(2) 0.5276(5) 0.26353(18) 0.0417(10) Uani 1 1 d .
H6 H 0.1082 0.4080 0.2716 0.050 Uiso 1 1 calc R
C11 C 0.0788(2) 0.6032(5) 0.19922(19) 0.0411(10) Uani 1 1 d .
H7 H 0.0881 0.5339 0.1644 0.049 Uiso 1 1 calc R
C12 C 0.05353(19) 0.7825(5) 0.18700(17) 0.0339(9) Uani 1 1 d .
C13 C 0.04002(19) 0.8811(5) 0.23931(17) 0.0389(10) Uani 1 1 d .
H8 H 0.0235 1.0021 0.2316 0.047 Uiso 1 1 calc R
C14 C 0.0503(2) 0.8049(5) 0.30315(18) 0.0394(10) Uani 1 1 d .
H9 H 0.0402 0.8742 0.3376 0.047 Uiso 1 1 calc R
C15 C 0.03620(19) 0.8633(6) 0.11662(18) 0.0348(9) Uani 1 1 d .
C16 C 0.0178(2) 0.3924(6) 0.3717(2) 0.0462(11) Uani 1 1 d .
C17 C 0.0826(2) 0.6581(7) 0.44289(18) 0.0454(11) Uani 1 1 d .
C18 C 0.6465(2) 0.3390(6) 0.42338(18) 0.0411(10) Uani 1 1 d .
C19 C 0.67545(19) 0.4769(5) 0.38387(18) 0.0343(9) Uani 1 1 d .
C20 C 0.7432(2) 0.4506(6) 0.37046(19) 0.0425(10) Uani 1 1 d .
H10 H 0.7736 0.3521 0.3900 0.051 Uiso 1 1 calc R
C21 C 0.7654(2) 0.5705(5) 0.3282(2) 0.0444(11) Uani 1 1 d .
H11 H 0.8103 0.5501 0.3187 0.053 Uiso 1 1 calc R
C22 C 0.7223(2) 0.7206(5) 0.29967(19) 0.0381(9) Uani 1 1 d .
C23 C 0.6569(2) 0.7515(5) 0.3164(2) 0.0494(11) Uani 1 1 d .
H12 H 0.6283 0.8551 0.2995 0.059 Uiso 1 1 calc R
C24 C 0.6335(2) 0.6312(6) 0.35786(19) 0.0455(11) Uani 1 1 d .
H13 H 0.5893 0.6537 0.3684 0.055 Uiso 1 1 calc R
C25 C 0.7500 0.8422(8) 0.2500 0.0439(14) Uani 1 2 d S
C26 C 0.6872(3) 0.9648(6) 0.2049(3) 0.0608(13) Uani 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'
Cu Cu 0.3201 1.2651 '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
O4 Cu O3 167.97(11) 2_545 4_666
O4 Cu O1 89.20(11) 2_545 .
O3 Cu O1 91.45(11) 4_666 .
O4 Cu O2 88.54(11) 2_545 3_656
O3 Cu O2 88.31(11) 4_666 3_656
O1 Cu O2 167.84(11) . 3_656
O4 Cu O5 92.06(10) 2_545 .
O3 Cu O5 99.61(10) 4_666 .
O1 Cu O5 100.81(10) . .
O2 Cu O5 91.21(9) 3_656 .
O4 Cu Cu 82.54(8) 2_545 3_656
O3 Cu Cu 85.48(8) 4_666 3_656
O1 Cu Cu 87.84(8) . 3_656
O2 Cu Cu 80.02(8) 3_656 3_656
O5 Cu Cu 169.77(7) . 3_656
C1 O1 Cu 120.9(2) . .
C1 O2 Cu 127.0(2) . 3_656
C15 O3 Cu 120.9(2) . 4_565
C15 O4 Cu 124.5(2) . 2_565
C18 O5 Cu 127.6(3) . .
O1 C1 O2 124.2(3) . .
O1 C1 C2 118.0(3) . .
O2 C1 C2 117.8(3) . .
C3 C2 C7 119.7(4) . .
C3 C2 C1 119.7(4) . .
C7 C2 C1 120.6(3) . .
C2 C3 C4 120.1(4) . .
C3 C4 C5 120.9(4) . .
C6 C5 C4 118.4(3) . .
C6 C5 C8 122.7(3) . .
C4 C5 C8 118.9(3) . .
C7 C6 C5 120.6(4) . .
C6 C7 C2 120.3(4) . .
C9 C8 C16 106.4(3) . .
C9 C8 C5 110.7(3) . .
C16 C8 C5 113.7(3) . .
C9 C8 C17 112.4(3) . .
C16 C8 C17 108.2(3) . .
C5 C8 C17 105.5(3) . .
C14 C9 C10 118.0(3) . .
C14 C9 C8 124.4(3) . .
C10 C9 C8 117.4(3) . .
C11 C10 C9 121.6(4) . .
C12 C11 C10 119.7(4) . .
C13 C12 C11 118.8(3) . .
C13 C12 C15 120.5(3) . .
C11 C12 C15 120.5(4) . .
C12 C13 C14 121.5(4) . .
C13 C14 C9 120.3(4) . .
O4 C15 O3 126.5(3) . .
O4 C15 C12 116.1(3) . .
O3 C15 C12 117.4(4) . .
F1 C16 F2 106.4(3) . .
F1 C16 F3 106.5(3) . .
F2 C16 F3 107.0(3) . .
F1 C16 C8 111.4(3) . .
F2 C16 C8 111.7(3) . .
F3 C16 C8 113.5(3) . .
F4 C17 F6 107.0(3) . .
F4 C17 F5 107.4(4) . .
F6 C17 F5 106.8(3) . .
F4 C17 C8 111.5(3) . .
F6 C17 C8 111.1(4) . .
F5 C17 C8 112.8(3) . .
O5 C18 O6 123.8(4) . .
O5 C18 C19 123.2(4) . .
O6 C18 C19 113.1(3) . .
C24 C19 C20 118.9(4) . .
C24 C19 C18 120.0(3) . .
C20 C19 C18 121.0(4) . .
C21 C20 C19 120.0(4) . .
C20 C21 C22 121.4(3) . .
C21 C22 C23 118.3(4) . .
C21 C22 C25 117.6(3) . .
C23 C22 C25 124.2(3) . .
C24 C23 C22 120.9(4) . .
C23 C24 C19 120.4(3) . .
C26 C25 C26 109.7(5) 2_655 .
C26 C25 C22 106.2(2) 2_655 .
C26 C25 C22 112.2(2) . .
C26 C25 C22 112.2(2) 2_655 2_655
C26 C25 C22 106.2(2) . 2_655
C22 C25 C22 110.3(4) . 2_655
F9 C26 F7 107.1(4) . .
F9 C26 F8 107.6(4) . .
F7 C26 F8 106.6(4) . .
F9 C26 C25 112.0(4) . .
F7 C26 C25 110.3(3) . .
F8 C26 C25 112.9(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O4 1.937(2) 2_545
Cu O3 1.939(2) 4_666
Cu O1 1.952(2) .
Cu O2 1.998(2) 3_656
Cu O5 2.207(3) .
Cu Cu 2.6446(10) 3_656
F1 C16 1.329(5) .
F2 C16 1.330(4) .
F3 C16 1.336(4) .
F4 C17 1.326(5) .
F5 C17 1.335(4) .
F6 C17 1.331(4) .
F7 C26 1.334(5) .
F8 C26 1.334(5) .
F9 C26 1.319(5) .
O1 C1 1.243(4) .
O2 C1 1.274(4) .
O2 Cu 1.998(2) 3_656
O3 C15 1.255(4) .
O3 Cu 1.939(2) 4_565
O4 C15 1.254(4) .
O4 Cu 1.937(2) 2_565
O5 C18 1.209(4) .
O6 C18 1.311(4) .
C1 C2 1.499(4) .
C2 C3 1.368(5) .
C2 C7 1.373(5) .
C3 C4 1.373(4) .
C4 C5 1.382(5) .
C5 C6 1.379(5) .
C5 C8 1.548(4) .
C6 C7 1.373(5) .
C8 C9 1.537(4) .
C8 C16 1.538(5) .
C8 C17 1.558(5) .
C9 C14 1.383(5) .
C9 C10 1.386(5) .
C10 C11 1.385(5) .
C11 C12 1.385(5) .
C12 C13 1.373(5) .
C12 C15 1.502(5) .
C13 C14 1.381(4) .
C18 C19 1.487(5) .
C19 C24 1.383(5) .
C19 C20 1.388(5) .
C20 C21 1.375(5) .
C21 C22 1.381(5) .
C22 C23 1.384(5) .
C22 C25 1.548(5) .
C23 C24 1.376(5) .
C25 C26 1.548(5) 2_655
C25 C26 1.548(5) .
C25 C22 1.548(5) 2_655
