#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:09:00 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180170 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/66/7106692.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_7106692
loop_
_publ_author_name
Christopher
B.
Caputo,
V.
Nicholas
Vukotic,
Natalie
M.
Sirizzotti
and
Stephen
J.
Loeb
'Christopher Caputo'
'V. Nicholas Vukotic'
'Natalie Sirizzotti'
'Stephen Loeb'
_publ_section_title
;
 A tetrapyridine ligand with a rigid tetrahedral core forms
 metal–organic frameworks with PtS type architecture
;
_journal_name_full               Chem.Commun.
_journal_page_first              8545
_journal_paper_doi               10.1039/c1cc12188j
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C64.5 H77.5 Cl2 Cu N10.5 O6.5'
_chemical_formula_weight         1238.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           50
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2b'
_symmetry_space_group_name_H-M   'P b a n :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            4
_cell_length_a                   14.995(3)
_cell_length_b                   30.625(7)
_cell_length_c                   14.689(3)
_cell_measurement_reflns_used    364
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.35
_cell_volume                     6746(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL XPREP'
_computing_molecular_graphics    'Bruker SHELXTL XP'
_computing_publication_material  'Bruker SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'phi and 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  0.1884
_diffrn_reflns_av_sigmaI/netI    0.1299
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            60393
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7739
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2612
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
The unit cell contains an estimated 26 molecules of DMF which have
been treated as a diffuse contribution to the overall scattering
without specific atom positions by SQUEEZE/PLATON.

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.

There was evidence of disorder at the Cu2-Cl2-N13 coordination envoronment.
The largest residual peak is close to Cu2 and there is evidence for
splitting peaks N13 - C18. All attempts to model this disorder with two
sets of CuCl(py) fragments resulted in unstable refinement and/or NPD atoms.
;
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1666
_refine_ls_R_factor_gt           0.0821
_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)+(0.0914P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                2853
_reflns_number_total             5946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12188j.txt
_cod_data_source_block           cc22o
_cod_original_sg_symbol_H-M      Pban
_cod_database_code               7106692
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z'
'x, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z'
'-x, y-1/2, z'
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
Cu1 Cu 1.7500 0.7500 0.5000 0.0662(5) Uani 1 4 d S . .
Cl1 Cl 1.7500 0.7500 0.6810(3) 0.1560(13) Uani 1 2 d S . .
N1 N 1.8460(2) 0.79685(10) 0.5034(3) 0.0516(10) Uani 1 1 d . . .
C2 C 1.9105(3) 0.79657(13) 0.4418(4) 0.0526(13) Uani 1 1 d . . .
H2A H 1.9122 0.7735 0.3987 0.063 Uiso 1 1 calc R . .
C3 C 1.9762(3) 0.82885(13) 0.4378(4) 0.0541(13) Uani 1 1 d . . .
H3A H 2.0215 0.8280 0.3927 0.065 Uiso 1 1 calc R . .
C4 C 1.9731(2) 0.86286(11) 0.5033(3) 0.0402(10) Uani 1 1 d . . .
C5 C 1.9071(3) 0.86077(13) 0.5669(3) 0.0503(12) Uani 1 1 d . . .
H5A H 1.9040 0.8821 0.6138 0.060 Uiso 1 1 calc R . .
C6 C 1.8462(3) 0.82849(12) 0.5633(3) 0.0512(13) Uani 1 1 d . . .
H6A H 1.8000 0.8287 0.6075 0.061 Uiso 1 1 calc R . .
C7 C 2.0407(2) 0.89818(11) 0.5039(3) 0.0335(9) Uani 1 1 d . . .
C8 C 2.0905(3) 0.90692(11) 0.4240(3) 0.0429(12) Uani 1 1 d . . .
H8A H 2.0803 0.8898 0.3710 0.052 Uiso 1 1 calc R . .
C9 C 2.1541(2) 0.94006(12) 0.4215(3) 0.0342(10) Uani 1 1 d . . .
H9A H 2.1872 0.9452 0.3674 0.041 Uiso 1 1 calc R . .
C10 C 2.1693(2) 0.96586(10) 0.4986(3) 0.0310(9) Uani 1 1 d . . .
C11 C 2.1195(2) 0.95703(11) 0.5755(3) 0.0338(10) Uani 1 1 d . . .
H11A H 2.1284 0.9740 0.6289 0.041 Uiso 1 1 calc R . .
C12 C 2.0568(2) 0.92393(12) 0.5760(3) 0.0351(10) Uani 1 1 d . . .
H12A H 2.0234 0.9192 0.6301 0.042 Uiso 1 1 calc R . .
N13 N 2.2523(7) 1.20119(14) 0.0946(4) 0.151(4) Uani 1 1 d . . .
C14 C 2.3236(7) 1.1930(2) 0.1477(5) 0.168(5) Uani 1 1 d . . .
H14A H 2.3737 1.2120 0.1448 0.202 Uiso 1 1 calc R . .
C15 C 2.3256(5) 1.1582(2) 0.2058(5) 0.125(3) Uani 1 1 d . . .
H15A H 2.3770 1.1532 0.2421 0.150 Uiso 1 1 calc R . .
C16 C 2.2543(5) 1.13032(14) 0.2123(3) 0.0820(18) Uani 1 1 d . . .
C17 C 2.1797(6) 1.1381(2) 0.1579(5) 0.145(3) Uani 1 1 d . . .
H17A H 2.1287 1.1197 0.1591 0.174 Uiso 1 1 calc R . .
C18 C 2.1851(8) 1.1750(3) 0.1012(5) 0.171(5) Uani 1 1 d . . .
H18A H 2.1347 1.1812 0.0642 0.205 Uiso 1 1 calc R . .
C19 C 2.2598(4) 1.09281(12) 0.2806(3) 0.0504(12) Uani 1 1 d . . .
C20 C 2.3302(3) 1.08657(13) 0.3384(3) 0.0515(13) Uani 1 1 d . . .
H20A H 2.3823 1.1040 0.3321 0.062 Uiso 1 1 calc R . .
C21 C 2.3262(3) 1.05527(12) 0.4055(3) 0.0421(11) Uani 1 1 d . . .
H21A H 2.3752 1.0520 0.4460 0.050 Uiso 1 1 calc R . .
C22 C 2.2526(3) 1.02839(10) 0.4154(3) 0.0324(9) Uani 1 1 d . . .
C23 C 2.1820(3) 1.03398(11) 0.3567(3) 0.0361(10) Uani 1 1 d . . .
H23A H 2.1308 1.0159 0.3630 0.043 Uiso 1 1 calc R . .
C24 C 2.1837(3) 1.06531(13) 0.2887(3) 0.0516(12) Uani 1 1 d . . .
H24A H 2.1348 1.0684 0.2480 0.062 Uiso 1 1 calc R . .
C25 C 2.2500 0.99697(14) 0.5000 0.0301(12) Uani 1 2 d S . .
Cu2 Cu 2.2500 1.2500 0.0000 0.244(2) Uani 1 4 d S . .
Cl2 Cl 2.4565(3) 1.2500 0.0000 0.1709(14) Uani 1 2 d S . .
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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
N1 Cu1 N1 90.20(18) 2_865 4_566 ?
N1 Cu1 N1 89.87(18) 2_865 3_856 ?
N1 Cu1 N1 177.2(2) 4_566 3_856 ?
N1 Cu1 N1 177.2(2) 2_865 . ?
N1 Cu1 N1 89.87(18) 4_566 . ?
N1 Cu1 N1 90.20(18) 3_856 . ?
N1 Cu1 Cl1 91.41(12) 2_865 3_856 ?
N1 Cu1 Cl1 88.59(12) 4_566 3_856 ?
N1 Cu1 Cl1 88.59(12) 3_856 3_856 ?
N1 Cu1 Cl1 91.41(12) . 3_856 ?
N1 Cu1 Cl1 88.59(12) 2_865 . ?
N1 Cu1 Cl1 91.41(12) 4_566 . ?
N1 Cu1 Cl1 91.41(12) 3_856 . ?
N1 Cu1 Cl1 88.59(12) . . ?
Cl1 Cu1 Cl1 180.000(1) 3_856 . ?
C6 N1 C2 117.5(3) . . ?
C6 N1 Cu1 122.8(3) . . ?
C2 N1 Cu1 119.7(3) . . ?
N1 C2 C3 122.7(4) . . ?
N1 C2 H2A 118.7 . . ?
C3 C2 H2A 118.7 . . ?
C2 C3 C4 117.9(4) . . ?
C2 C3 H3A 121.0 . . ?
C4 C3 H3A 121.0 . . ?
C5 C4 C3 117.0(4) . . ?
C5 C4 C7 121.8(4) . . ?
C3 C4 C7 121.2(4) . . ?
C6 C5 C4 120.0(4) . . ?
C6 C5 H5A 120.0 . . ?
C4 C5 H5A 120.0 . . ?
N1 C6 C5 124.9(4) . . ?
N1 C6 H6A 117.6 . . ?
C5 C6 H6A 117.6 . . ?
C12 C7 C8 116.6(3) . . ?
C12 C7 C4 123.9(4) . . ?
C8 C7 C4 119.5(4) . . ?
C9 C8 C7 121.3(4) . . ?
C9 C8 H8A 119.3 . . ?
C7 C8 H8A 119.3 . . ?
C8 C9 C10 120.1(4) . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C11 C10 C9 117.6(3) . . ?
C11 C10 C25 122.4(3) . . ?
C9 C10 C25 119.2(3) . . ?
C10 C11 C12 121.1(4) . . ?
C10 C11 H11A 119.5 . . ?
C12 C11 H11A 119.5 . . ?
C7 C12 C11 123.3(4) . . ?
C7 C12 H12A 118.4 . . ?
C11 C12 H12A 118.4 . . ?
C18 N13 C14 117.4(6) . . ?
C18 N13 Cu2 119.6(8) . . ?
C14 N13 Cu2 122.9(7) . . ?
N13 C14 C15 121.6(8) . . ?
N13 C14 H14A 119.2 . . ?
C15 C14 H14A 119.2 . . ?
C14 C15 C16 120.8(7) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C15 C16 C17 118.7(5) . . ?
C15 C16 C19 118.1(6) . . ?
C17 C16 C19 123.2(6) . . ?
C16 C17 C18 115.5(8) . . ?
C16 C17 H17A 122.3 . . ?
C18 C17 H17A 122.3 . . ?
N13 C18 C17 126.1(9) . . ?
N13 C18 H18A 116.9 . . ?
C17 C18 H18A 116.9 . . ?
C20 C19 C24 119.0(4) . . ?
C20 C19 C16 123.7(5) . . ?
C24 C19 C16 117.1(5) . . ?
C19 C20 C21 120.5(4) . . ?
C19 C20 H20A 119.7 . . ?
C21 C20 H20A 119.7 . . ?
C20 C21 C22 121.6(4) . . ?
C20 C21 H21A 119.2 . . ?
C22 C21 H21A 119.2 . . ?
C23 C22 C21 118.2(3) . . ?
C23 C22 C25 123.5(3) . . ?
C21 C22 C25 117.8(3) . . ?
C22 C23 C24 121.6(4) . . ?
C22 C23 H23A 119.2 . . ?
C24 C23 H23A 119.2 . . ?
C23 C24 C19 118.9(4) . . ?
C23 C24 H24A 120.5 . . ?
C19 C24 H24A 120.5 . . ?
C10 C25 C10 103.6(4) . 3_956 ?
C10 C25 C22 111.7(2) . 3_956 ?
C10 C25 C22 112.8(2) 3_956 3_956 ?
C10 C25 C22 112.8(2) . . ?
C10 C25 C22 111.7(2) 3_956 . ?
C22 C25 C22 104.5(4) 3_956 . ?
N13 Cu2 N13 85.8(3) . 3_955 ?
N13 Cu2 N13 94.2(3) . 2_975 ?
N13 Cu2 N13 178.1(6) 3_955 2_975 ?
N13 Cu2 N13 178.1(6) . 4_575 ?
N13 Cu2 N13 94.2(3) 3_955 4_575 ?
N13 Cu2 N13 85.8(3) 2_975 4_575 ?
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
Cu1 N1 2.032(3) 2_865 ?
Cu1 N1 2.032(3) 4_566 ?
Cu1 N1 2.032(3) 3_856 ?
Cu1 N1 2.032(3) . ?
Cu1 Cl1 2.658(4) 3_856 ?
Cu1 Cl1 2.658(4) . ?
N1 C6 1.308(5) . ?
N1 C2 1.325(5) . ?
C2 C3 1.397(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.418(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.363(5) . ?
C4 C7 1.483(5) . ?
C5 C6 1.347(5) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 C12 1.342(5) . ?
C7 C8 1.417(5) . ?
C8 C9 1.393(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.400(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.380(5) . ?
C10 C25 1.540(4) . ?
C11 C12 1.383(5) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
N13 C18 1.292(13) . ?
N13 C14 1.347(12) . ?
N13 Cu2 2.041(5) . ?
C14 C15 1.367(8) . ?
C14 H14A 0.9500 . ?
C15 C16 1.371(8) . ?
C15 H15A 0.9500 . ?
C16 C17 1.395(9) . ?
C16 C19 1.528(6) . ?
C17 C18 1.406(9) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 C20 1.367(6) . ?
C19 C24 1.424(6) . ?
C20 C21 1.376(5) . ?
C20 H20A 0.9500 . ?
C21 C22 1.385(5) . ?
C21 H21A 0.9500 . ?
C22 C23 1.377(5) . ?
C22 C25 1.572(4) . ?
C23 C24 1.386(5) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
C25 C10 1.540(4) 3_956 ?
C25 C22 1.572(4) 3_956 ?
Cu2 N13 2.041(5) 3_955 ?
Cu2 N13 2.041(5) 2_975 ?
Cu2 N13 2.041(5) 4_575 ?
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 -0.001 -0.003 -0.006 3787 1866
;
;
