#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:18:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178777 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/31/4103187.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_4103187
loop_
_publ_author_name
'Jennifer K. Schnobrich'
'Olivier Lebel'
'Katie A. Cychosz'
'Anne Dailly'
'Antek G. Wong-Foy'
'Adam J. Matzger'
_publ_section_title
;
 Linker-Directed Vertex Desymmetrization for the Production of
 Coordination Polymers with High Porosity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13941
_journal_page_last               13948
_journal_paper_doi               10.1021/ja107423k
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C14 H7 Cu O5'
_chemical_formula_sum            'C14 H7 Cu O5'
_chemical_formula_weight         318.74
_chemical_name_common            UMCM-153
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                90.00
_cell_formula_units_Z            32
_cell_length_a                   21.7064(7)
_cell_length_b                   29.0072(11)
_cell_length_c                   43.700(3)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.42
_cell_measurement_theta_min      6.51
_cell_volume                     27515(2)
_computing_cell_refinement       FS-Process
_computing_data_collection       'CrystalClear (Version 2.0)'
_computing_data_reduction        'CrystalClear (Version 4.0) '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1197
_diffrn_reflns_av_sigmaI/netI    0.1194
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            15770
_diffrn_reflns_theta_full        50.42
_diffrn_reflns_theta_max         50.42
_diffrn_reflns_theta_min         6.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_correction_T_min  0.8166
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
  Higashi, T. (1995). Program for Absorption Correction.
  Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            blade
_exptl_crystal_density_diffrn    0.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blue
_exptl_crystal_F_000             5120
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0768
_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)+(0.1096P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                2291
_reflns_number_total             3591
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107423k_si_001_3.cif
_cod_data_source_block           UMCM-153
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4103187
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/4, -y+3/4, z+1/2'
'x, y+1/2, z+1/2'
'-x, y+3/4, z+3/4'
'x+1/4, -y+1/2, z+3/4'
'-x+1/4, -y+5/4, z+1'
'x+1/2, y, z+1/2'
'-x+1/2, y+1/4, z+3/4'
'x+3/4, -y, z+3/4'
'-x+3/4, -y+3/4, z+1'
'x+1/2, y+1/2, z'
'-x+1/2, y+3/4, z+1/4'
'x+3/4, -y+1/2, z+1/4'
'-x+3/4, -y+5/4, z+1/2'
'-x, -y, -z'
'x, -y-1/4, -z-1/4'
'-x-1/4, y, -z-1/4'
'x-1/4, y-3/4, -z-1/2'
'-x, -y+1/2, -z+1/2'
'x, -y+1/4, -z+1/4'
'-x-1/4, y+1/2, -z+1/4'
'x-1/4, y-1/4, -z'
'-x+1/2, -y, -z+1/2'
'x+1/2, -y-1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x+1/4, y-3/4, -z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/4, -z-1/4'
'-x+1/4, y+1/2, -z-1/4'
'x+1/4, y-1/4, -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
Cu1 Cu -0.00087(3) 0.52870(3) 0.023090(17) 0.0461(5) Uani 1 1 d .
O2 O 0.07769(16) 0.50064(15) 0.03318(9) 0.0635(13) Uani 1 1 d .
O3 O 0.04364(16) 0.52039(15) -0.04584(8) 0.0593(12) Uani 1 1 d .
O19 O 0.08015(15) 0.45079(14) -0.00685(9) 0.0630(13) Uani 1 1 d .
O20 O 0.00119(17) 0.57962(16) 0.06285(9) 0.0943(15) Uani 1 1 d .
O21 O 0.04236(16) 0.56772(12) -0.00595(9) 0.0551(11) Uani 1 1 d .
C4 C 0.1636(2) 0.4499(2) 0.02905(14) 0.0546(17) Uani 1 1 d .
C5 C 0.1912(3) 0.4126(2) 0.01495(13) 0.0666(19) Uani 1 1 d .
H5 H 0.1740 0.3997 -0.0026 0.080 Uiso 1 1 calc R
C6 C 0.2440(3) 0.4530(3) 0.06526(16) 0.082(2) Uani 1 1 d .
H6 H 0.2629 0.4675 0.0818 0.098 Uiso 1 1 calc R
C7 C 0.2699(3) 0.4141(2) 0.05297(15) 0.0638(19) Uani 1 1 d .
C8 C 0.2444(3) 0.3947(3) 0.02723(13) 0.069(2) Uani 1 1 d .
H8 H 0.2633 0.3694 0.0181 0.083 Uiso 1 1 calc R
C9 C 0.1895(3) 0.4712(2) 0.05319(14) 0.0613(18) Uani 1 1 d .
H9 H 0.1715 0.4974 0.0617 0.074 Uiso 1 1 calc R
C10 C 0.3261(2) 0.3940(2) 0.06987(14) 0.0625(19) Uani 1 1 d .
C11 C 0.3750 0.3750 0.05415(19) 0.073(3) Uani 1 2 d S
H11 H 0.3750 0.3750 0.0329 0.087 Uiso 1 2 calc SR
C12 C 0.3252(2) 0.3943(2) 0.10103(13) 0.0609(19) Uani 1 1 d .
H12 H 0.2921 0.4071 0.1114 0.073 Uiso 1 1 calc R
C13 C 0.3750 0.3750 0.11750(18) 0.062(3) Uani 1 2 d S
C14 C 0.3750 0.3750 0.1501(2) 0.059(3) Uani 1 2 d S
C15 C 0.3443(2) 0.4083(2) 0.16820(14) 0.0534(17) Uani 1 1 d .
H15 H 0.3241 0.4322 0.1582 0.064 Uiso 1 1 calc R
C16 C 0.3750 0.3750 0.21646(19) 0.055(2) Uani 1 2 d S
H16 H 0.3750 0.3750 0.2377 0.066 Uiso 1 2 calc SR
C17 C 0.3424(2) 0.4073(2) 0.19966(14) 0.0478(16) Uani 1 1 d .
C18 C 0.1006(3) 0.4696(2) 0.01763(17) 0.0555(18) Uani 1 1 d .
C22 C 0.0564(3) 0.5579(3) -0.03315(17) 0.057(2) 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 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 '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 O21 88.19(16) . .
O2 Cu1 O19 169.78(16) . 17_565
O21 Cu1 O19 90.61(15) . 17_565
O2 Cu1 O3 89.78(16) . 17_565
O21 Cu1 O3 168.25(16) . 17_565
O19 Cu1 O3 89.33(16) 17_565 17_565
O2 Cu1 O20 94.66(16) . .
O21 Cu1 O20 96.37(16) . .
O19 Cu1 O20 95.55(16) 17_565 .
O3 Cu1 O20 95.33(17) 17_565 .
O2 Cu1 Cu1 84.01(13) . 17_565
O21 Cu1 Cu1 81.95(12) . 17_565
O19 Cu1 Cu1 85.78(13) 17_565 17_565
O3 Cu1 Cu1 86.33(14) 17_565 17_565
O20 Cu1 Cu1 177.88(11) . 17_565
C18 O2 Cu1 122.4(4) . .
C22 O3 Cu1 120.6(4) . 17_565
C18 O19 Cu1 118.6(4) . 17_565
C22 O21 Cu1 127.0(4) . .
C9 C4 C5 121.9(6) . .
C9 C4 C18 116.6(6) . .
C5 C4 C18 121.4(6) . .
C8 C5 C4 119.0(6) . .
C8 C5 H5 120.5 . .
C4 C5 H5 120.5 . .
C7 C6 C9 120.6(6) . .
C7 C6 H6 119.7 . .
C9 C6 H6 119.7 . .
C6 C7 C8 119.5(6) . .
C6 C7 C10 116.7(6) . .
C8 C7 C10 123.7(6) . .
C7 C8 C5 120.2(6) . .
C7 C8 H8 119.9 . .
C5 C8 H8 119.9 . .
C4 C9 C6 118.4(6) . .
C4 C9 H9 120.8 . .
C6 C9 H9 120.8 . .
C12 C10 C11 120.7(6) . .
C12 C10 C7 117.8(5) . .
C11 C10 C7 121.5(6) . .
C10 C11 C10 120.3(8) 12_554 .
C10 C11 H11 119.9 12_554 .
C10 C11 H11 119.9 . .
C10 C12 C13 119.8(6) . .
C10 C12 H12 120.1 . .
C13 C12 H12 120.1 . .
C12 C13 C12 118.8(7) . 12_554
C12 C13 C14 120.6(4) . .
C12 C13 C14 120.6(4) 12_554 .
C15 C14 C15 112.0(8) . 12_554
C15 C14 C13 124.0(4) . .
C15 C14 C13 124.0(4) 12_554 .
C17 C15 C14 124.1(6) . .
C17 C15 H15 118.0 . .
C14 C15 H15 118.0 . .
C17 C16 C17 116.0(8) . 12_554
C17 C16 H16 122.0 . .
C17 C16 H16 122.0 12_554 .
C15 C17 C16 121.8(6) . .
C15 C17 C22 120.7(6) . 3_565
C16 C17 C22 117.5(6) . 3_565
O2 C18 O19 129.1(6) . .
O2 C18 C4 116.3(7) . .
O19 C18 C4 114.5(7) . .
O3 C22 O21 124.1(7) . .
O3 C22 C17 119.0(6) . 11_464
O21 C22 C17 116.9(6) . 11_464
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.940(4) .
Cu1 O21 1.942(4) .
Cu1 O19 1.954(3) 17_565
Cu1 O3 1.969(4) 17_565
Cu1 O20 2.281(4) .
Cu1 Cu1 2.6165(15) 17_565
O2 C18 1.233(7) .
O3 C22 1.252(6) .
O3 Cu1 1.969(4) 17_565
O19 C18 1.281(7) .
O19 Cu1 1.954(3) 17_565
O21 C22 1.260(6) .
C4 C9 1.345(7) .
C4 C5 1.383(7) .
C4 C18 1.564(7) .
C5 C8 1.375(7) .
C5 H5 0.9300 .
C6 C7 1.370(8) .
C6 C9 1.399(7) .
C6 H6 0.9300 .
C7 C8 1.374(7) .
C7 C10 1.540(7) .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 C12 1.362(6) .
C10 C11 1.380(6) .
C11 C10 1.380(6) 12_554
C11 H11 0.9300 .
C12 C13 1.413(6) .
C12 H12 0.9300 .
C13 C12 1.413(6) 12_554
C13 C14 1.425(9) .
C14 C15 1.414(6) .
C14 C15 1.414(6) 12_554
C15 C17 1.376(6) .
C15 H15 0.9300 .
C16 C17 1.386(6) .
C16 C17 1.386(6) 12_554
C16 H16 0.9300 .
C17 C22 1.480(8) 3_565
C22 C17 1.480(8) 11_464
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O21 Cu1 O2 C18 -82.3(5) . .
O19 Cu1 O2 C18 1.1(12) 17_565 .
O3 Cu1 O2 C18 86.1(5) 17_565 .
O20 Cu1 O2 C18 -178.6(5) . .
Cu1 Cu1 O2 C18 -0.2(4) 17_565 .
O2 Cu1 O21 C22 84.6(4) . .
O19 Cu1 O21 C22 -85.2(4) 17_565 .
O3 Cu1 O21 C22 4.5(10) 17_565 .
O20 Cu1 O21 C22 179.1(4) . .
Cu1 Cu1 O21 C22 0.4(4) 17_565 .
C9 C4 C5 C8 4.4(9) . .
C18 C4 C5 C8 -175.6(5) . .
C9 C6 C7 C8 4.6(10) . .
C9 C6 C7 C10 -173.8(6) . .
C6 C7 C8 C5 -3.9(10) . .
C10 C7 C8 C5 174.4(6) . .
C4 C5 C8 C7 -0.5(9) . .
C5 C4 C9 C6 -3.7(9) . .
C18 C4 C9 C6 176.3(5) . .
C7 C6 C9 C4 -0.8(9) . .
C6 C7 C10 C12 39.2(9) . .
C8 C7 C10 C12 -139.2(7) . .
C6 C7 C10 C11 -142.5(6) . .
C8 C7 C10 C11 39.1(9) . .
C12 C10 C11 C10 0.0(4) . 12_554
C7 C10 C11 C10 -178.3(6) . 12_554
C11 C10 C12 C13 0.0(9) . .
C7 C10 C12 C13 178.3(5) . .
C10 C12 C13 C12 0.0(4) . 12_554
C10 C12 C13 C14 -180.0(4) . .
C12 C13 C14 C15 -28.0(4) . .
C12 C13 C14 C15 152.0(4) 12_554 .
C12 C13 C14 C15 152.0(4) . 12_554
C12 C13 C14 C15 -28.0(4) 12_554 12_554
C15 C14 C15 C17 -2.5(4) 12_554 .
C13 C14 C15 C17 177.5(4) . .
C14 C15 C17 C16 5.1(8) . .
C14 C15 C17 C22 -176.8(4) . 3_565
C17 C16 C17 C15 -2.4(4) 12_554 .
C17 C16 C17 C22 179.4(5) 12_554 3_565
Cu1 O2 C18 O19 1.0(9) . .
Cu1 O2 C18 C4 -179.0(3) . .
Cu1 O19 C18 O2 -1.3(8) 17_565 .
Cu1 O19 C18 C4 178.7(3) 17_565 .
C9 C4 C18 O2 -5.4(8) . .
C5 C4 C18 O2 174.6(5) . .
C9 C4 C18 O19 174.6(5) . .
C5 C4 C18 O19 -5.4(8) . .
Cu1 O3 C22 O21 -1.7(7) 17_565 .
Cu1 O3 C22 C17 175.8(3) 17_565 11_464
Cu1 O21 C22 O3 0.6(8) . .
Cu1 O21 C22 C17 -177.0(3) . 11_464
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
_platon_squeeze_void_content
1 -0.002 -0.007 -0.002 19946 3371 ' '
