#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/05/7220567.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_7220567
loop_
_publ_author_name
'Díaz-Gallifa, P.'
'Fabelo, O.'
'Pasán, J.'
'Cañadillas-Delgado, L.'
'Ramírez, M. A.'
'Gallardo, A. G.'
'Ruiz-Pérez, C.'
_publ_section_title
;
 Synthesis and structural characterization of six Cu(ii)-based
 coordination polymers using the thermally tunable
 1,2,3,4-cyclobutanetetracarboxylic acid
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              5081
_journal_paper_doi               10.1039/C5CE00326A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C16 H8 Cu4 O21'
_chemical_formula_weight         790.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-06 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                110.768(8)
_cell_angle_beta                 96.370(8)
_cell_angle_gamma                97.671(7)
_cell_formula_units_Z            2
_cell_length_a                   8.0007(8)
_cell_length_b                   11.0476(9)
_cell_length_c                   14.0408(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1133.12(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7596
_diffrn_reflns_theta_full        71.91
_diffrn_reflns_theta_max         71.91
_diffrn_reflns_theta_min         4.36
_exptl_absorpt_coefficient_mu    5.244
_exptl_absorpt_correction_T_max  0.5231
_exptl_absorpt_correction_T_min  0.4820
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    2.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.1000
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0498
_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)+(0.0859P)²+2.1843P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1490
_reflns_number_gt                3608
_reflns_number_total             4405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00326a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7220563--7220567.cif.
;
_cod_original_cell_volume        1133.12(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7220567
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t_ave  0.5030
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Cu1 Cu 0.61735(8) 0.63031(6) 0.23110(5) 0.02221(19) Uani 1 1 d .
Cu2 Cu 0.71096(8) 0.94243(6) 0.26347(5) 0.02081(19) Uani 1 1 d .
Cu3 Cu 0.76720(8) 1.22854(6) 0.25432(5) 0.01964(19) Uani 1 1 d .
Cu4 Cu 0.16483(8) 1.28362(6) 0.24884(5) 0.02081(19) Uani 1 1 d .
O1 O 0.2843(7) 0.6225(5) 0.1080(6) 0.083(2) Uani 1 1 d .
O2 O 0.5176(4) 0.7650(3) 0.1939(3) 0.0260(7) Uani 1 1 d .
O3 O 0.6049(4) 1.0612(3) 0.2091(2) 0.0198(6) Uani 1 1 d .
O4 O 0.4202(5) 1.1928(3) 0.2096(3) 0.0353(9) Uani 1 1 d .
O5 O -0.1352(4) 0.9163(3) 0.1570(3) 0.0266(7) Uani 1 1 d .
O6 O 0.0110(4) 1.1206(3) 0.2395(3) 0.0222(7) Uani 1 1 d .
O7 O -0.0630(4) 0.7504(3) -0.1066(3) 0.0253(7) Uani 1 1 d .
O8 O 0.2190(4) 0.7923(4) -0.1114(3) 0.0263(7) Uani 1 1 d .
O9 O 1.0614(5) 0.9477(4) 0.3686(4) 0.0496(12) Uani 1 1 d .
O10 O 0.8035(4) 0.8195(3) 0.3155(3) 0.0246(7) Uani 1 1 d .
O11 O 0.7289(4) 0.5022(3) 0.2698(3) 0.0279(7) Uani 1 1 d .
O12 O 0.9258(4) 0.3946(3) 0.3025(3) 0.0214(6) Uani 1 1 d .
O13 O 1.3139(4) 0.4475(3) 0.2572(3) 0.0252(7) Uani 1 1 d .
O14 O 1.4682(4) 0.6485(3) 0.3340(3) 0.0265(7) Uani 1 1 d .
O15 O 1.2467(4) 0.7423(3) 0.6017(2) 0.0250(7) Uani 1 1 d .
O16 O 1.2951(5) 0.9441(3) 0.5949(3) 0.0331(8) Uani 1 1 d .
C1 C 0.3196(6) 0.8343(4) 0.0975(4) 0.0219(9) Uani 1 1 d .
H1 H 0.3946 0.8487 0.0503 0.026 Uiso 1 1 calc R
C2 C 0.3718(7) 0.7313(5) 0.1343(4) 0.0300(11) Uani 1 1 d .
C3 C 0.3081(6) 0.9688(4) 0.1806(3) 0.0206(9) Uani 1 1 d .
H3 H 0.2874 0.9589 0.2452 0.025 Uiso 1 1 calc R
C4 C 0.4472(6) 1.0826(5) 0.2011(4) 0.0213(9) Uani 1 1 d .
C5 C 0.1369(5) 0.9666(4) 0.1143(3) 0.0188(9) Uani 1 1 d .
H5 H 0.1562 1.0205 0.0727 0.023 Uiso 1 1 calc R
C6 C -0.0074(6) 1.0028(5) 0.1740(4) 0.0218(9) Uani 1 1 d .
C7 C 0.1316(6) 0.8184(4) 0.0493(3) 0.0195(9) Uani 1 1 d .
H7 H 0.0548 0.7607 0.0715 0.023 Uiso 1 1 calc R
C8 C 0.0942(6) 0.7816(4) -0.0665(3) 0.0204(9) Uani 1 1 d .
C9 C 1.0170(5) 0.7462(4) 0.3982(3) 0.0189(8) Uani 1 1 d .
H9 H 0.9480 0.7348 0.4489 0.023 Uiso 1 1 calc R
C10 C 0.9636(6) 0.8487(4) 0.3600(4) 0.0239(10) Uani 1 1 d .
C11 C 1.0250(5) 0.6108(4) 0.3154(3) 0.0182(8) Uani 1 1 d .
H11 H 1.0452 0.6206 0.2507 0.022 Uiso 1 1 calc R
C12 C 0.8827(6) 0.4964(4) 0.2942(3) 0.0186(8) Uani 1 1 d .
C13 C 1.1969(5) 0.6124(4) 0.3802(3) 0.0173(8) Uani 1 1 d .
H13 H 1.1768 0.5646 0.4260 0.021 Uiso 1 1 calc R
C14 C 1.3351(6) 0.5652(4) 0.3196(3) 0.0189(8) Uani 1 1 d .
C15 C 1.2111(6) 0.7620(4) 0.4390(3) 0.0192(9) Uani 1 1 d .
H15 H 1.2812 0.8124 0.4078 0.023 Uiso 1 1 calc R
C16 C 1.2571(6) 0.8208(4) 0.5547(4) 0.0200(9) Uani 1 1 d .
O1W O 0.2497(5) 1.3170(4) 0.3943(3) 0.0348(8) Uani 1 1 d .
O2W O 0.7079(7) 0.5809(5) 0.1020(4) 0.0573(13) Uani 1 1 d .
O1X O 0.3395(6) 1.1392(5) 0.4639(4) 0.0488(11) Uani 1 1 d .
O2X O 0.4195(9) 1.5343(7) 0.5555(6) 0.0329(16) Uani 0.50 1 d P
O3X O -0.3887(9) 0.6838(8) -0.0360(6) 0.088(2) Uani 1 1 d .
O4X O 0.0393(12) 0.5097(10) -0.0502(8) 0.053(2) Uani 0.50 1 d P
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'
Cu Cu -1.9646 0.5888 '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'
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
O14 Cu1 O2W 163.8(2) 1_455 .
O14 Cu1 O11 92.97(16) 1_455 .
O2W Cu1 O11 90.47(19) . .
O14 Cu1 O2 88.68(16) 1_455 .
O2W Cu1 O2 88.66(19) . .
O11 Cu1 O2 176.93(14) . .
O14 Cu1 O10 97.76(14) 1_455 .
O2W Cu1 O10 96.9(2) . .
O11 Cu1 O10 102.70(13) . .
O2 Cu1 O10 74.49(13) . .
O10 Cu2 O16 89.17(15) . 2_776
O10 Cu2 O3 176.94(13) . .
O16 Cu2 O3 91.26(15) 2_776 .
O10 Cu2 O5 92.32(15) . 1_655
O16 Cu2 O5 140.38(16) 2_776 1_655
O3 Cu2 O5 89.28(15) . 1_655
O10 Cu2 O2 76.85(13) . .
O16 Cu2 O2 117.18(16) 2_776 .
O3 Cu2 O2 100.28(13) . .
O5 Cu2 O2 101.64(14) 1_655 .
O12 Cu3 O15 88.17(14) 1_565 2_776
O12 Cu3 O8 89.89(15) 1_565 2_675
O15 Cu3 O8 177.44(15) 2_776 2_675
O12 Cu3 O3 178.51(14) 1_565 .
O15 Cu3 O3 90.37(14) 2_776 .
O8 Cu3 O3 91.55(14) 2_675 .
O12 Cu3 O6 87.84(12) 1_565 1_655
O15 Cu3 O6 98.38(14) 2_776 1_655
O8 Cu3 O6 83.21(13) 2_675 1_655
O3 Cu3 O6 92.66(12) . 1_655
O7 Cu4 O1W 175.67(16) 2_575 .
O7 Cu4 O13 90.85(15) 2_575 1_465
O1W Cu4 O13 91.64(16) . 1_465
O7 Cu4 O6 88.42(14) 2_575 .
O1W Cu4 O6 89.03(15) . .
O13 Cu4 O6 178.79(14) 1_465 .
O7 Cu4 O4 96.97(15) 2_575 .
O1W Cu4 O4 86.88(16) . .
O13 Cu4 O4 82.11(13) 1_465 .
O6 Cu4 O4 98.94(13) . .
C2 O2 Cu1 119.2(3) . .
C2 O2 Cu2 135.8(3) . .
Cu1 O2 Cu2 104.86(14) . .
C4 O3 Cu3 109.9(3) . .
C4 O3 Cu2 131.4(3) . .
Cu3 O3 Cu2 107.99(14) . .
C4 O4 Cu4 128.3(3) . .
C6 O5 Cu2 118.2(3) . 1_455
C6 O6 Cu4 129.5(3) . .
C6 O6 Cu3 118.8(3) . 1_455
Cu4 O6 Cu3 91.69(13) . 1_455
C8 O7 Cu4 128.1(3) . 2_575
C8 O8 Cu3 132.0(3) . 2_675
C10 O10 Cu2 119.0(3) . .
C10 O10 Cu1 134.0(3) . .
Cu2 O10 Cu1 103.21(14) . .
C12 O11 Cu1 133.2(3) . .
C12 O12 Cu3 121.9(3) . 1_545
C14 O13 Cu4 132.0(3) . 1_645
C14 O14 Cu1 122.2(3) . 1_655
C16 O15 Cu3 131.5(3) . 2_776
C16 O16 Cu2 127.8(3) . 2_776
C2 C1 C7 119.1(4) . .
C2 C1 C3 117.5(4) . .
C7 C1 C3 89.9(3) . .
O1 C2 O2 122.4(5) . .
O1 C2 C1 122.4(5) . .
O2 C2 C1 115.2(4) . .
C4 C3 C1 118.0(4) . .
C4 C3 C5 116.0(4) . .
C1 C3 C5 88.7(3) . .
O4 C4 O3 120.1(4) . .
O4 C4 C3 122.9(4) . .
O3 C4 C3 116.9(4) . .
C6 C5 C7 118.2(4) . .
C6 C5 C3 115.2(4) . .
C7 C5 C3 89.0(3) . .
O5 C6 O6 124.0(4) . .
O5 C6 C5 118.2(4) . .
O6 C6 C5 117.7(4) . .
C8 C7 C1 116.5(4) . .
C8 C7 C5 114.6(4) . .
C1 C7 C5 89.2(3) . .
O8 C8 O7 126.9(4) . .
O8 C8 C7 117.4(4) . .
O7 C8 C7 115.5(4) . .
C10 C9 C11 117.1(4) . .
C10 C9 C15 117.3(4) . .
C11 C9 C15 88.8(3) . .
O9 C10 O10 123.8(5) . .
O9 C10 C9 123.0(4) . .
O10 C10 C9 113.3(4) . .
C12 C11 C9 118.9(4) . .
C12 C11 C13 116.8(4) . .
C9 C11 C13 88.5(3) . .
O11 C12 O12 121.9(4) . .
O11 C12 C11 121.7(4) . .
O12 C12 C11 116.4(4) . .
C14 C13 C15 118.6(4) . .
C14 C13 C11 115.9(4) . .
C15 C13 C11 89.0(3) . .
O14 C14 O13 123.0(4) . .
O14 C14 C13 116.9(4) . .
O13 C14 C13 120.2(4) . .
C16 C15 C13 120.3(4) . .
C16 C15 C9 113.6(4) . .
C13 C15 C9 88.7(3) . .
O16 C16 O15 126.6(4) . .
O16 C16 C15 116.1(4) . .
O15 C16 C15 117.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O14 1.947(3) 1_455
Cu1 O2W 1.950(5) .
Cu1 O11 1.967(3) .
Cu1 O2 1.975(3) .
Cu1 O10 2.239(3) .
Cu2 O10 1.944(3) .
Cu2 O16 1.949(4) 2_776
Cu2 O3 1.972(3) .
Cu2 O5 2.007(3) 1_655
Cu2 O2 2.165(3) .
Cu3 O12 1.935(3) 1_565
Cu3 O15 1.950(3) 2_776
Cu3 O8 1.954(3) 2_675
Cu3 O3 1.963(3) .
Cu3 O6 2.409(3) 1_655
Cu4 O7 1.954(3) 2_575
Cu4 O1W 1.964(4) .
Cu4 O13 1.989(3) 1_465
Cu4 O6 1.995(3) .
Cu4 O4 2.427(4) .
O1 C2 1.214(7) .
O2 C2 1.283(6) .
O3 C4 1.314(5) .
O4 C4 1.232(6) .
O5 C6 1.241(6) .
O5 Cu2 2.007(3) 1_455
O6 C6 1.278(6) .
O6 Cu3 2.409(3) 1_455
O7 C8 1.267(6) .
O7 Cu4 1.954(3) 2_575
O8 C8 1.254(6) .
O8 Cu3 1.954(3) 2_675
O9 C10 1.216(6) .
O10 C10 1.305(6) .
O11 C12 1.257(6) .
O12 C12 1.258(6) .
O12 Cu3 1.935(3) 1_545
O13 C14 1.260(6) .
O13 Cu4 1.989(3) 1_645
O14 C14 1.258(6) .
O14 Cu1 1.947(3) 1_655
O15 C16 1.262(6) .
O15 Cu3 1.950(3) 2_776
O16 C16 1.254(6) .
O16 Cu2 1.949(4) 2_776
C1 C2 1.494(7) .
C1 C7 1.540(6) .
C1 C3 1.553(6) .
C3 C4 1.484(6) .
C3 C5 1.560(6) .
C5 C6 1.515(6) .
C5 C7 1.558(6) .
C7 C8 1.513(6) .
C9 C10 1.505(7) .
C9 C11 1.549(6) .
C9 C15 1.558(6) .
C11 C12 1.503(6) .
C11 C13 1.557(6) .
C13 C14 1.505(6) .
C13 C15 1.545(6) .
C15 C16 1.500(6) .
O4X O4X 1.67(2) 2_565
