#------------------------------------------------------------------------------
#$Date: 2017-11-17 03:41:21 +0100 (vie 17 de nov de 2017) $
#$Revision: 203243 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/95/7229584.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_7229584
loop_
_publ_author_name
'Patil, Komal M.'
'Telfer, Shane'
'Moratti, Stephen'
'Qazvini, Omid T.'
'Hanton, Lyall R.'
_publ_section_title
;
 A Non-Interpenetrated Cu-based MOF Constructed from a Rediscovered
 Tetrahedral Ligand
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01818E
_journal_year                    2017
_chemical_formula_moiety         '(C19 H14 Cu O4)(H2O)(C3 H7 N O)7'
_chemical_formula_sum            'C40 H64 Cu N7 O12'
_chemical_formula_weight         898.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_Hall           '-P 4c 2'
_space_group_name_H-M_alt        'P 42/m m c'
_symmetry_space_group_name_Hall  '-P 4c 2'
_symmetry_space_group_name_H-M   'P 42/m m c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-07-31 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.686(5)
_cell_length_b                   14.686(5)
_cell_length_c                   26.103(9)
_cell_measurement_reflns_used    407
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      63.2950
_cell_measurement_theta_min      4.2600
_cell_volume                     5630(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-T (Sheldrick, 2014)'
_diffrn_ambient_environment      N2
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1725
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.3040
_diffrn_reflns_av_unetI/netI     0.1438
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22352
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.952
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.2064
_exptl_crystal_size_mid          0.1329
_exptl_crystal_size_min          0.0883
_platon_squeeze_details
;
The PLATON SQUEEZE procedure was used to treat regions of diffuse
solvent which could not be sensibly modelled in terms of atomic
sites. Their contribution to the diffraction pattern was removed
and modified F(obs)**2 written to a new HKL file. 
Total electron count is 1905 electrons in a total void volume of 4486 Å³.
The number of electrons thus located are included in the
formula, formula weight, calculated density, mu and F(000).
This residual electron density was assigned to 7 molecules of DMF per Cu(II)
cation
[1905/4 = 291.25 e per asymmetric unit; DMF = 56 e]
;
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         2826
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.3011
_refine_ls_R_factor_gt           0.1642
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1500P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4208
_refine_ls_wR_factor_ref         0.5026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                625
_reflns_number_total             2826
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce01818e2.cif
_cod_data_source_block           UOF_1A
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        5630(5)
_cod_database_code               7229584
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
_shelx_res_file
;
TITL shelxt_a.res in P4(2)/mmc
CELL  1.54184  14.6861  14.6861  26.1026   90.000   90.000   90.000
ZERR     8.00   0.0053   0.0053   0.0090    0.000    0.000    0.000
LATT   1
SYMM  - X, - Y,   Z
SYMM  - Y,   X, 1/2 + Z
SYMM    Y, - X, 1/2 + Z
SYMM  - X,   Y, - Z
SYMM    X, - Y, - Z
SYMM    Y,   X, 1/2 - Z
SYMM  - Y, - X, 1/2 - Z
SFAC  C    H    O    CU
UNIT  76 56 20 4
MERG   2
OMIT    -2 136
OMIT     0   4   1
OMIT     0   3   2
OMIT     1   3   2
OMIT     0   1   4
OMIT     0   2   5
OMIT     1   3   3
OMIT     0   4   5
OMIT     0   4   0
OMIT     1   3   6
OMIT     2   4   0
OMIT     1   4   0
OMIT     1   3   4
OMIT     1   2   6
OMIT     1   2   5
OMIT     1   4   2
DFIX 1.35 0.02 C1 C2
FMAP   2
PLAN   20
BOND   $H
BOND
ACTA
LIST   6
L.S.  10
WGHT    0.150000
FVAR      27.39723
C1    1    0.885352    0.500000    0.436474    10.50000    0.09391
C2    1    0.812087    0.500000    0.396680    10.50000    0.18292
C3    1    0.785865    0.425324    0.374075    11.00000    0.23361
AFIX  43
H3    2    0.819623    0.372714    0.379773    11.00000   -1.20000
AFIX   0
C4    1    0.699345    0.418594    0.337199    11.00000    0.21397
AFIX  43
H4    2    0.671909    0.363544    0.328726    11.00000   -1.20000
AFIX   0
C5    1    0.669184    0.500000    0.319245    10.50000    0.15199
C6    1    0.586073    0.500000    0.282124    10.50000    0.09055
C7    1    0.582763    0.417237    0.250000    10.50000    0.10396
AFIX  23
H7A   2    0.584415    0.363917    0.271911    10.50000   -1.20000
H7B   2    0.636085    0.415582    0.228090    10.50000   -1.20000
AFIX   0
C8    1    0.500000    0.500000    0.314833    10.25000    0.10588
AFIX  23
H8A   2    0.500001    0.446594    0.336698    10.25000   -1.20000
H8B   2    0.500001    0.553406    0.336698    10.25000   -1.20000
AFIX   0
O1    3    0.904026    0.579439    0.447776    11.00000    0.13458
O2    3    1.000000    0.736699    0.500000    10.25000    0.20914
CU1   4    1.000000    0.587784    0.500000    10.25000    0.13988    0.24636 =
         0.07383    0.00000    0.00000    0.00000
HKLF    4

REM  shelxt_a.res in P4(2)/mmc
REM R1 =  0.1642 for     625 Fo > 4sig(Fo)  and  0.3011 for all    2826 data
REM     35 parameters refined using      1 restraints

END

WGHT      0.1727      0.0000

REM Highest difference peak  0.589,  deepest hole -0.877,  1-sigma level  0.082
Q1    1   1.0000  0.5413  0.5000  10.25000  0.05    0.59
Q2    1   1.0535  0.5854  0.5000  10.50000  0.05    0.54
Q3    1   1.0000  0.6300  0.5000  10.25000  0.05    0.46
Q4    1   0.7211  0.5000  0.3139  10.50000  0.05    0.46
Q5    1   0.7534  0.5000  0.3940  10.50000  0.05    0.45
Q6    1   0.9159  0.5000  0.4412  10.50000  0.05    0.37
Q7    1   0.5879  0.3640  0.2557  11.00000  0.05    0.36
Q8    1   0.8217  0.4136  0.3529  11.00000  0.05    0.31
Q9    1   1.0000  0.7493  0.4637  10.50000  0.05    0.27
Q10   1   0.6439  0.4131  0.3572  11.00000  0.05    0.26
Q11   1   0.9039  0.6533  0.4438  11.00000  0.05    0.24
Q12   1   1.0644  0.7494  0.5000  10.50000  0.05    0.23
Q13   1   0.7242  0.3433  0.3138  11.00000  0.05    0.18
Q14   1   0.5765  0.5000  0.5000  10.25000  0.05    0.16
Q15   1   0.7800  0.3422  0.3855  11.00000  0.05    0.15
Q16   1   0.6532  0.5000  0.2112  10.50000  0.05    0.11
Q17   1   0.5000  0.1482  0.4090  10.50000  0.05    0.10
Q18   1   1.0000  0.9208  0.4129  10.50000  0.05    0.10
Q19   1   0.5000  0.0000  0.5000  10.12500  0.05    0.09
Q20   1   1.0000  0.9333  0.3567  10.50000  0.05    0.09
;
_shelx_res_checksum              90319
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z+1/2'
'y, -x, z+1/2'
'-x, y, -z'
'x, -y, -z'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z-1/2'
'-y, x, -z-1/2'
'x, -y, z'
'-x, y, z'
'-y, -x, z-1/2'
'y, x, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.8854(8) 0.5000 0.4365(4) 0.094(3) Uiso 1 2 d DS . P
C2 C 0.8121(13) 0.5000 0.3967(7) 0.183(8) Uiso 1 2 d DS . P
C3 C 0.7859(13) 0.4253(12) 0.3741(7) 0.234(8) Uiso 1 1 d . . .
H3 H 0.8196 0.3727 0.3798 0.280 Uiso 1 1 calc R U .
C4 C 0.6993(12) 0.4186(11) 0.3372(6) 0.214(6) Uiso 1 1 d . . .
H4 H 0.6719 0.3635 0.3287 0.257 Uiso 1 1 calc R U .
C5 C 0.6692(12) 0.5000 0.3192(6) 0.152(6) Uiso 1 2 d S . P
C6 C 0.5861(8) 0.5000 0.2821(4) 0.091(3) Uiso 1 2 d S . P
C7 C 0.5828(6) 0.4172(6) 0.2500 0.104(3) Uiso 1 2 d S . P
H7A H 0.5844 0.3639 0.2719 0.125 Uiso 0.5 1 calc R U P
H7B H 0.6361 0.4156 0.2281 0.125 Uiso 0.5 1 calc R U P
C8 C 0.5000 0.5000 0.3148(6) 0.106(5) Uiso 1 4 d S . P
H8A H 0.5000 0.4466 0.3367 0.127 Uiso 0.5 2 calc R U P
H8B H 0.5000 0.5534 0.3367 0.127 Uiso 0.5 2 calc R U P
O1 O 0.9040(5) 0.5794(5) 0.4478(3) 0.135(2) Uiso 1 1 d . . .
O2 O 1.0000 0.7367(14) 0.5000 0.209(8) Uiso 1 4 d S . P
Cu1 Cu 1.0000 0.5878(3) 0.5000 0.1534(19) Uani 1 4 d S T 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 0.140(3) 0.246(5) 0.0738(14) 0.000 0.000 0.000
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
O1 C1 O1 141.9(13) . 13_565
O1 C1 C2 109.0(6) . .
O1 C1 C2 109.0(6) 13_565 .
C3 C2 C3 115(2) 13_565 .
C3 C2 C1 121.8(12) 13_565 .
C3 C2 C1 121.8(12) . .
C2 C3 C4 124.0(18) . .
C2 C3 H3 118.0 . .
C4 C3 H3 118.0 . .
C5 C4 C3 114.4(17) . .
C5 C4 H4 122.8 . .
C3 C4 H4 122.8 . .
C4 C5 C4 123(2) . 13_565
C4 C5 C6 118.0(12) . .
C4 C5 C6 118.0(12) 13_565 .
C7 C6 C7 110.7(8) 12_656 .
C7 C6 C8 106.9(7) 12_656 .
C7 C6 C8 106.9(7) . .
C7 C6 C5 112.3(7) 12_656 .
C7 C6 C5 112.3(7) . .
C8 C6 C5 107.5(9) . .
C6 C7 C6 112.1(12) . 11_566
C6 C7 H7A 109.2 . .
C6 C7 H7A 109.2 11_566 .
C6 C7 H7B 109.2 . .
C6 C7 H7B 109.2 11_566 .
H7A C7 H7B 107.9 . .
C6 C8 C6 111.9(13) 2_665 .
C6 C8 H8A 109.2 2_665 .
C6 C8 H8A 109.2 . .
C6 C8 H8B 109.2 2_665 .
C6 C8 H8B 109.2 . .
H8A C8 H8B 107.9 . .
C1 O1 Cu1 112.6(8) . .
O1 Cu1 O1 87.9(4) 5_756 14_755
O1 Cu1 O1 91.7(4) 5_756 10_556
O1 Cu1 O1 172.9(5) 14_755 10_556
O1 Cu1 O1 172.8(5) 5_756 .
O1 Cu1 O1 91.7(4) 14_755 .
O1 Cu1 O1 87.9(4) 10_556 .
O1 Cu1 O2 93.6(2) 5_756 .
O1 Cu1 O2 93.6(2) 14_755 .
O1 Cu1 O2 93.6(2) 10_556 .
O1 Cu1 O2 93.6(2) . .
O1 Cu1 Cu1 86.4(2) 5_756 9_766
O1 Cu1 Cu1 86.4(2) 14_755 9_766
O1 Cu1 Cu1 86.4(2) 10_556 9_766
O1 Cu1 Cu1 86.4(2) . 9_766
O2 Cu1 Cu1 180.0 . 9_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.234(7) .
C1 O1 1.234(7) 13_565
C1 C2 1.496(15) .
C2 C3 1.304(18) 13_565
C2 C3 1.304(18) .
C3 C4 1.60(2) .
C3 H3 0.9300 .
C4 C5 1.358(15) .
C4 H4 0.9300 .
C5 C4 1.358(15) 13_565
C5 C6 1.558(19) .
C6 C7 1.477(8) 12_656
C6 C7 1.477(8) .
C6 C8 1.525(13) .
C7 C6 1.477(8) 11_566
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C6 1.525(13) 2_665
C8 H8A 0.9700 .
C8 H8B 0.9700 .
O1 Cu1 1.965(7) .
O2 Cu1 2.19(2) .
Cu1 O1 1.965(7) 5_756
Cu1 O1 1.965(7) 14_755
Cu1 O1 1.965(7) 10_556
Cu1 Cu1 2.578(9) 9_766
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 -0.018 -0.006 -0.006 4486 1905 ' '
