 
data_uhouston05
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 uhouston05
;
_chemical_name_common             CTHMOF342
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C14 H2 Cu F8 N8 O'
_chemical_formula_weight          513.78
 
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'
 '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'
 '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'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    C2/m
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'
 
_cell_length_a                    15.8991(10)
_cell_length_b                    31.5712(18)
_cell_length_c                    13.8721(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  115.357(3)
_cell_angle_gamma                 90.00
_cell_volume                      6292.3(6)
_cell_formula_units_Z             8
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     9971
_cell_measurement_theta_min       2.40
_cell_measurement_theta_max       25.32
 
_exptl_crystal_description        block
_exptl_crystal_colour             blue
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.085
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2008
_exptl_absorpt_coefficient_mu     0.756
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9148
_exptl_absorpt_correction_T_max   0.9704
_exptl_absorpt_process_details    SADABS

_diffrn_refln_scan_width					1.0
_diffrn_refln_scan_rate						20
_space_group.centring_type				C-centered
_space_group.IT_number						12

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  0.000  0.000 -0.024      1699       655 'unk diff solvent'
   2  0.500  0.500 -0.039      1699       655 'unk diff solvent'
_platon_squeeze_details
;
;
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'microfocus sealed tube'
_diffrn_radiation_monochromator   'QUAZAR multilayer mirrors'
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'phi and omega scans'
_diffrn_detector_area_resol_mean  8.366
_diffrn_reflns_number             37915
_diffrn_reflns_av_R_equivalents   0.0693
_diffrn_reflns_av_sigmaI/netI     0.0576
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -37
_diffrn_reflns_limit_k_max        36
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          1.56
_diffrn_reflns_theta_max          25.43
_reflns_number_total              5907
_reflns_number_gt                 4454
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SIR-97'
_computing_structure_refinement   'SHELXL-97'
_computing_molecular_graphics     'ORTEP-32'
_computing_publication_material   'WinGX'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.1509P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5907
_refine_ls_number_parameters      303
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.0896
_refine_ls_R_factor_gt            0.0753
_refine_ls_wR_factor_ref          0.2346
_refine_ls_wR_factor_gt           0.2272
_refine_ls_goodness_of_fit_ref    1.119
_refine_ls_restrained_S_all       1.119
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
C1 C 0.3618(3) 0.09995(13) 0.3154(3) 0.0250(10) Uani 1 1 d . . .
C2 C 0.3168(4) 0.14201(15) 0.2920(4) 0.0398(13) Uani 1 1 d . . .
C3 C 0.2518(4) 0.15358(16) 0.3278(4) 0.0396(12) Uani 1 1 d . . .
C4 C 0.2093(4) 0.19291(15) 0.3049(4) 0.0463(14) Uani 1 1 d . . .
C5 C 0.2348(5) 0.22229(19) 0.2475(5) 0.0639(19) Uani 1 1 d . . .
C6 C 0.2943(8) 0.2104(2) 0.2131(7) 0.103(4) Uani 1 1 d . . .
C7 C 0.3401(7) 0.1721(2) 0.2355(7) 0.095(3) Uani 1 1 d . . .
C8 C 0.6044(3) 0.10359(14) 0.1809(3) 0.0303(11) Uani 1 1 d . . .
C9 C 0.6340(4) 0.14745(14) 0.1978(4) 0.0405(13) Uani 1 1 d . . .
C10 C 0.6742(4) 0.16647(16) 0.2983(4) 0.0410(13) Uani 1 1 d . . .
C11 C 0.7007(4) 0.20751(19) 0.3137(4) 0.0511(15) Uani 1 1 d . . .
C12 C 0.6954(5) 0.23386(17) 0.2303(5) 0.0608(19) Uani 1 1 d . . .
C13 C 0.6557(6) 0.21560(19) 0.1313(5) 0.078(2) Uani 1 1 d . . .
C14 C 0.6267(6) 0.17412(19) 0.1153(5) 0.075(2) Uani 1 1 d . . .
N1 N 0.4321(3) 0.04569(11) 0.3935(3) 0.0233(8) Uani 1 1 d . . .
N2 N 0.4237(3) 0.04440(10) 0.2945(3) 0.0222(8) Uani 1 1 d . . .
N3 N 0.3809(3) 0.07808(10) 0.2426(3) 0.0281(9) Uani 1 1 d . . .
N4 N 0.3932(3) 0.08020(11) 0.4089(3) 0.0294(9) Uani 1 1 d . . .
N5 N 0.5469(2) 0.04567(10) 0.1990(3) 0.0198(8) Uani 1 1 d . . .
N6 N 0.5572(3) 0.04540(10) 0.1101(3) 0.0229(8) Uani 1 1 d . . .
N7 N 0.5929(3) 0.08075(11) 0.0954(3) 0.0319(9) Uani 1 1 d . . .
N8 N 0.5776(3) 0.08241(11) 0.2470(3) 0.0287(9) Uani 1 1 d . . .
O1 O 0.6041(3) 0.0000 0.4227(3) 0.0226(9) Uani 1 2 d SD . .
O2 O 0.3790(3) 0.0000 0.0620(3) 0.0227(9) Uani 1 2 d SD . .
F1 F 0.2232(2) 0.12615(9) 0.3797(3) 0.0551(9) Uani 1 1 d . . .
F2 F 0.1441(2) 0.20198(9) 0.3391(3) 0.0568(9) Uani 1 1 d . . .
F3 F 0.3290(6) 0.23929(13) 0.1615(6) 0.177(4) Uani 1 1 d . . .
F4 F 0.4033(5) 0.16262(12) 0.1988(5) 0.135(3) Uani 1 1 d . . .
F5 F 0.6848(2) 0.14305(8) 0.3847(2) 0.0491(8) Uani 1 1 d . . .
F6 F 0.7420(3) 0.22212(10) 0.4151(2) 0.0586(9) Uani 1 1 d . . .
F7 F 0.6466(6) 0.23904(13) 0.0485(3) 0.167(3) Uani 1 1 d . . .
F8 F 0.5954(4) 0.15877(11) 0.0175(3) 0.115(2) Uani 1 1 d . . .
Cu1 Cu 0.5000 0.0000 0.5000 0.0165(3) Uani 1 4 d S . .
Cu2 Cu 0.48423(5) 0.0000 0.24330(5) 0.0186(2) Uani 1 2 d S . .
Cu3 Cu 0.5000 0.0000 0.0000 0.0192(3) Uani 1 4 d S . .
H1 H 0.6395(8) -0.02208(8) 0.436(3) 0.023 Uiso 1 1 d D . .
H2 H 0.3469(12) 0.02215(8) 0.035(3) 0.023 Uiso 1 1 d D . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
C1 N4 1.329(5) . ?
C1 N3 1.361(5) . ?
C1 C2 1.476(6) . ?
C2 C3 1.375(7) . ?
C2 C7 1.379(8) . ?
C3 F1 1.325(6) . ?
C3 C4 1.384(7) . ?
C4 F2 1.343(6) . ?
C4 C5 1.391(8) . ?
C5 C6 1.284(10) . ?
C5 C12 1.496(8) 8_455 ?
C6 C7 1.379(9) . ?
C6 F3 1.409(8) . ?
C7 F4 1.340(7) . ?
C8 N7 1.332(6) . ?
C8 N8 1.344(5) . ?
C8 C9 1.449(6) . ?
C9 C14 1.386(7) . ?
C9 C10 1.396(7) . ?
C10 C11 1.351(7) . ?
C10 F5 1.357(5) . ?
C11 F6 1.353(6) . ?
C11 C12 1.398(8) . ?
C12 C13 1.369(8) . ?
C12 C5 1.496(8) 8 ?
C13 F7 1.321(7) . ?
C13 C14 1.374(8) . ?
C14 F8 1.320(6) . ?
N1 N4 1.315(5) . ?
N1 N2 1.321(5) . ?
N1 Cu1 2.016(3) . ?
N2 N3 1.301(5) . ?
N2 Cu2 1.995(3) . ?
N5 N6 1.312(4) . ?
N5 N8 1.323(5) . ?
N5 Cu2 1.994(3) . ?
N6 N7 1.306(5) . ?
N6 Cu3 2.006(3) . ?
O1 Cu1 2.326(4) . ?
O1 Cu2 2.400(4) . ?
O1 H1 0.865(5) . ?
O2 Cu2 2.350(4) . ?
O2 Cu3 2.421(4) . ?
O2 H2 0.853(5) . ?
Cu1 N1 2.016(3) 6 ?
Cu1 N1 2.016(3) 2_656 ?
Cu1 N1 2.016(3) 5_656 ?
Cu1 O1 2.326(4) 5_656 ?
Cu2 N5 1.994(3) 6 ?
Cu2 N2 1.995(3) 6 ?
Cu3 N6 2.006(3) 5_655 ?
Cu3 N6 2.006(3) 6 ?
Cu3 N6 2.006(3) 2_655 ?
Cu3 O2 2.421(4) 5_655 ?
 
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
N4 C1 N3 112.1(4) . . ?
N4 C1 C2 125.5(4) . . ?
N3 C1 C2 122.3(4) . . ?
C3 C2 C7 116.7(4) . . ?
C3 C2 C1 121.8(4) . . ?
C7 C2 C1 121.5(5) . . ?
F1 C3 C2 120.6(4) . . ?
F1 C3 C4 117.6(4) . . ?
C2 C3 C4 121.6(5) . . ?
F2 C4 C3 119.0(5) . . ?
F2 C4 C5 121.2(4) . . ?
C3 C4 C5 119.8(5) . . ?
C6 C5 C4 117.4(5) . . ?
C6 C5 C12 122.4(6) . 8_455 ?
C4 C5 C12 120.2(5) . 8_455 ?
C5 C6 C7 125.1(6) . . ?
C5 C6 F3 120.8(6) . . ?
C7 C6 F3 113.5(7) . . ?
F4 C7 C2 119.3(5) . . ?
F4 C7 C6 121.3(6) . . ?
C2 C7 C6 119.2(6) . . ?
N7 C8 N8 112.1(4) . . ?
N7 C8 C9 125.0(4) . . ?
N8 C8 C9 122.7(4) . . ?
C14 C9 C10 113.8(4) . . ?
C14 C9 C8 122.7(4) . . ?
C10 C9 C8 123.4(4) . . ?
C11 C10 F5 118.1(4) . . ?
C11 C10 C9 123.3(5) . . ?
F5 C10 C9 118.6(4) . . ?
C10 C11 F6 118.1(5) . . ?
C10 C11 C12 122.4(5) . . ?
F6 C11 C12 119.2(5) . . ?
C13 C12 C11 114.7(5) . . ?
C13 C12 C5 122.1(5) . 8 ?
C11 C12 C5 123.1(5) . 8 ?
F7 C13 C12 117.9(5) . . ?
F7 C13 C14 119.3(5) . . ?
C12 C13 C14 122.8(5) . . ?
F8 C14 C13 118.0(5) . . ?
F8 C14 C9 119.1(4) . . ?
C13 C14 C9 122.8(5) . . ?
N4 N1 N2 110.5(3) . . ?
N4 N1 Cu1 128.0(3) . . ?
N2 N1 Cu1 121.6(3) . . ?
N3 N2 N1 110.3(3) . . ?
N3 N2 Cu2 126.5(3) . . ?
N1 N2 Cu2 122.8(3) . . ?
N2 N3 C1 103.5(3) . . ?
N1 N4 C1 103.7(3) . . ?
N6 N5 N8 108.2(3) . . ?
N6 N5 Cu2 124.4(2) . . ?
N8 N5 Cu2 127.2(3) . . ?
N7 N6 N5 112.2(3) . . ?
N7 N6 Cu3 125.3(3) . . ?
N5 N6 Cu3 121.4(3) . . ?
N6 N7 C8 103.2(3) . . ?
N5 N8 C8 104.4(3) . . ?
Cu1 O1 Cu2 94.14(15) . . ?
Cu1 O1 H1 115(2) . . ?
Cu2 O1 H1 112(2) . . ?
Cu2 O2 Cu3 94.02(14) . . ?
Cu2 O2 H2 119.5(18) . . ?
Cu3 O2 H2 105(3) . . ?
N1 Cu1 N1 180.00(13) 6 2_656 ?
N1 Cu1 N1 91.36(19) 6 . ?
N1 Cu1 N1 88.64(19) 2_656 . ?
N1 Cu1 N1 88.64(19) 6 5_656 ?
N1 Cu1 N1 91.36(19) 2_656 5_656 ?
N1 Cu1 N1 180.00(13) . 5_656 ?
N1 Cu1 O1 85.73(13) 6 . ?
N1 Cu1 O1 94.27(13) 2_656 . ?
N1 Cu1 O1 85.73(13) . . ?
N1 Cu1 O1 94.27(13) 5_656 . ?
N1 Cu1 O1 94.27(13) 6 5_656 ?
N1 Cu1 O1 85.73(13) 2_656 5_656 ?
N1 Cu1 O1 94.27(13) . 5_656 ?
N1 Cu1 O1 85.73(13) 5_656 5_656 ?
O1 Cu1 O1 180.0 . 5_656 ?
N5 Cu2 N5 92.64(18) . 6 ?
N5 Cu2 N2 177.24(12) . 6 ?
N5 Cu2 N2 89.00(14) 6 6 ?
N5 Cu2 N2 89.00(14) . . ?
N5 Cu2 N2 177.24(12) 6 . ?
N2 Cu2 N2 89.27(19) 6 . ?
N5 Cu2 O2 83.73(12) . . ?
N5 Cu2 O2 83.73(12) 6 . ?
N2 Cu2 O2 98.65(12) 6 . ?
N2 Cu2 O2 98.65(12) . . ?
N5 Cu2 O1 92.28(12) . . ?
N5 Cu2 O1 92.28(12) 6 . ?
N2 Cu2 O1 85.44(12) 6 . ?
N2 Cu2 O1 85.44(12) . . ?
O2 Cu2 O1 174.21(13) . . ?
N6 Cu3 N6 180.0(2) . 5_655 ?
N6 Cu3 N6 91.20(19) . 6 ?
N6 Cu3 N6 88.80(19) 5_655 6 ?
N6 Cu3 N6 88.80(19) . 2_655 ?
N6 Cu3 N6 91.20(19) 5_655 2_655 ?
N6 Cu3 N6 180.0(4) 6 2_655 ?
N6 Cu3 O2 84.28(12) . . ?
N6 Cu3 O2 95.72(12) 5_655 . ?
N6 Cu3 O2 84.28(12) 6 . ?
N6 Cu3 O2 95.72(12) 2_655 . ?
N6 Cu3 O2 95.72(12) . 5_655 ?
N6 Cu3 O2 84.28(12) 5_655 5_655 ?
N6 Cu3 O2 95.72(12) 6 5_655 ?
N6 Cu3 O2 84.28(12) 2_655 5_655 ?
O2 Cu3 O2 180.00(14) . 5_655 ?
 
_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    1.809
_refine_diff_density_min   -0.897
_refine_diff_density_rms    0.118

