#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/05/7220563.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_7220563
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 H25 Cu5 O33'
_chemical_formula_weight         1063.06
_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                106.807(4)
_cell_angle_beta                 90.983(3)
_cell_angle_gamma                110.054(2)
_cell_formula_units_Z            1
_cell_length_a                   8.7022(3)
_cell_length_b                   8.9520(3)
_cell_length_c                   12.6698(6)
_cell_measurement_temperature    293(2)
_cell_volume                     880.10(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       KappaCCD
_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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8527
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         5.03
_exptl_absorpt_coefficient_mu    3.089
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8614
_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            blue
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_size_rad          0.0200
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3975
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0342
_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)+(0.0385P)²+1.7930P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                3323
_reflns_number_total             3975
_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_sg_symbol_H-M      P-1
_cod_database_code               7220563
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t_ave  0.8616
#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 0.0000 0.0000 0.0000 0.01801(14) Uani 1 2 d S
Cu2 Cu 0.01194(5) 0.04353(5) 0.33241(3) 0.01468(11) Uani 1 1 d .
Cu3 Cu -0.33935(5) 0.05522(5) 0.34359(3) 0.01414(11) Uani 1 1 d .
O1 O -0.2225(3) 0.2511(3) 0.3003(2) 0.0258(6) Uani 1 1 d .
O2 O 0.0370(3) 0.2636(3) 0.3207(2) 0.0214(5) Uani 1 1 d .
O3 O 0.0167(3) 0.2312(3) 0.0741(2) 0.0228(5) Uani 1 1 d .
O4 O 0.2897(3) 0.3607(4) 0.1086(3) 0.0460(9) Uani 1 1 d .
O5 O 0.3742(3) 0.8247(4) 0.2088(2) 0.0362(7) Uani 1 1 d .
O6 O 0.5021(3) 0.8554(3) 0.3695(2) 0.0215(5) Uani 1 1 d .
OH1 O -0.2115(3) -0.0636(3) 0.25930(18) 0.0153(5) Uani 1 1 d D
O7 O 0.0189(3) 0.8247(3) 0.33327(19) 0.0195(5) Uani 1 1 d .
O8 O 0.1642(3) 0.8975(3) 0.49817(18) 0.0205(5) Uani 1 1 d .
C1 C -0.0113(4) 0.4841(4) 0.2766(3) 0.0123(6) Uani 1 1 d .
H1 H -0.1024 0.5150 0.2559 0.019 Uiso 1 1 calc R
C2 C -0.0697(4) 0.3194(4) 0.2999(3) 0.0131(6) Uani 1 1 d .
C3 C 0.1236(4) 0.5067(4) 0.1983(3) 0.0146(6) Uani 1 1 d .
H2 H 0.1090 0.5763 0.1548 0.018 Uiso 1 1 calc R
C4 C 0.1465(4) 0.3550(4) 0.1222(3) 0.0212(7) Uani 1 1 d .
C5 C 0.2574(4) 0.6162(4) 0.2980(3) 0.0134(6) Uani 1 1 d .
H4 H 0.3135 0.5484 0.3182 0.016 Uiso 1 1 calc R
C6 C 0.3839(4) 0.7757(4) 0.2890(3) 0.0168(6) Uani 1 1 d .
C7 C 0.1166(4) 0.6264(4) 0.3736(2) 0.0113(6) Uani 1 1 d .
H3 H 0.1275 0.5907 0.4386 0.014 Uiso 1 1 calc R
C8 C 0.0968(4) 0.7943(4) 0.4044(3) 0.0129(6) Uani 1 1 d .
O1W O -0.4513(3) 0.1967(2) 0.4345(4) 0.0214(5) Uani 1 1 d .
O2W O 0.2168(3) 0.1606(3) 0.4367(2) 0.0216(5) Uani 1 1 d D
O3W O 0.1451(4) -0.0032(4) 0.1712(2) 0.0366(7) Uani 1 1 d D
O4W O 0.2196(3) 0.0686(3) -0.0490(2) 0.0227(5) Uani 1 1 d D
O1X O 0.4478(8) 0.2092(13) 0.2131(8) 0.085(3) Uani 0.50 1 d P
O2X O 0.7275(6) 0.3256(7) 0.0356(3) 0.0945(19) Uani 1 1 d .
O3X O 0.6256(4) 0.5693(4) 0.1848(3) 0.0524(9) Uani 1 1 d .
O4X O 0.3316(5) 0.4554(4) 0.5898(3) 0.0606(10) Uani 1 1 d .
H5 H 0.210(6) 0.067(7) -0.1236(16) 0.051(15) Uiso 1 1 d D
H6 H 0.278(5) 0.182(2) -0.009(3) 0.037(12) Uiso 1 1 d D
H7 H 0.129(12) -0.119(3) 0.148(8) 0.05(3) Uiso 0.50 1 d PD
H8 H 0.244(4) 0.090(4) 0.200(4) 0.059(17) Uiso 1 1 d D
H9 H 0.198(7) 0.097(6) 0.486(4) 0.066(17) Uiso 1 1 d D
H10 H 0.249(6) 0.271(3) 0.485(3) 0.056(15) Uiso 1 1 d D
H11 H -0.4637 0.1615 0.5020 0.09(2) Uiso 1 1 d .
H12 H -0.5488 0.2060 0.4130 0.063(17) Uiso 1 1 d .
H13 H -0.258(5) -0.1638(17) 0.248(4) 0.032(12) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 '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'
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
O3 Cu1 O3 180.0(2) . 2
O3 Cu1 O4W 93.64(10) . .
O3 Cu1 O4W 86.36(10) 2 .
O3 Cu1 O4W 86.36(10) . 2
O3 Cu1 O4W 93.64(10) 2 2
O4W Cu1 O4W 180.00(13) . 2
OH1 Cu2 O2 94.65(10) . .
OH1 Cu2 O2W 167.47(10) . .
O2 Cu2 O2W 86.03(10) . .
OH1 Cu2 O7 90.84(10) . 1_545
O2 Cu2 O7 170.98(10) . 1_545
O2W Cu2 O7 90.17(10) . 1_545
OH1 Cu2 O3W 97.39(11) . .
O2 Cu2 O3W 88.31(11) . .
O2W Cu2 O3W 95.13(11) . .
O7 Cu2 O3W 83.88(10) 1_545 .
OH1 Cu3 O1 90.69(10) . .
OH1 Cu3 O6 94.34(10) . 1_445
O1 Cu3 O6 168.08(11) . 1_445
OH1 Cu3 O1W 174.52(7) . .
O1 Cu3 O1W 85.06(7) . .
O6 Cu3 O1W 90.50(7) 1_445 .
OH1 Cu3 O8 87.00(9) . 2_566
O1 Cu3 O8 100.68(10) . 2_566
O6 Cu3 O8 90.39(9) 1_445 2_566
O1W Cu3 O8 90.41(6) . 2_566
C2 O1 Cu3 128.7(2) . .
C2 O2 Cu2 130.2(2) . .
C4 O3 Cu1 126.8(2) . .
C6 O6 Cu3 111.2(2) . 1_665
Cu3 OH1 Cu2 107.22(11) . .
C8 O7 Cu2 128.4(2) . 1_565
C8 O8 Cu3 143.5(2) . 2_566
C2 C1 C3 115.8(2) . .
C2 C1 C7 111.9(2) . .
C3 C1 C7 89.0(2) . .
O2 C2 O1 125.2(3) . .
O2 C2 C1 117.8(3) . .
O1 C2 C1 117.0(3) . .
C4 C3 C5 117.3(3) . .
C4 C3 C1 119.4(3) . .
C5 C3 C1 90.9(2) . .
O4 C4 O3 124.8(3) . .
O4 C4 C3 118.4(3) . .
O3 C4 C3 116.7(3) . .
C6 C5 C3 117.9(3) . .
C6 C5 C7 119.5(2) . .
C3 C5 C7 88.8(2) . .
O5 C6 O6 122.4(3) . .
O5 C6 C5 121.8(3) . .
O6 C6 C5 115.9(3) . .
C8 C7 C1 115.6(2) . .
C8 C7 C5 113.4(2) . .
C1 C7 C5 88.8(2) . .
O8 C8 O7 124.0(3) . .
O8 C8 C7 117.7(3) . .
O7 C8 C7 118.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O3 1.962(2) .
Cu1 O3 1.962(2) 2
Cu1 O4W 1.967(2) .
Cu1 O4W 1.967(2) 2
Cu2 OH1 1.925(2) .
Cu2 O2 1.956(2) .
Cu2 O2W 1.964(2) .
Cu2 O7 1.984(2) 1_545
Cu2 O3W 2.368(3) .
Cu3 OH1 1.925(2) .
Cu3 O1 1.939(2) .
Cu3 O6 1.968(2) 1_445
Cu3 O1W 1.980(3) .
Cu3 O8 2.342(2) 2_566
O1 C2 1.260(4) .
O2 C2 1.251(4) .
O3 C4 1.267(4) .
O4 C4 1.247(4) .
O5 C6 1.229(4) .
O6 C6 1.284(4) .
O6 Cu3 1.968(2) 1_665
O7 C8 1.262(4) .
O7 Cu2 1.984(2) 1_565
O8 C8 1.257(4) .
O8 Cu3 2.342(2) 2_566
C1 C2 1.504(4) .
C1 C3 1.548(4) .
C1 C7 1.564(4) .
C3 C4 1.499(4) .
C3 C5 1.537(4) .
C5 C6 1.512(4) .
C5 C7 1.579(4) .
C7 C8 1.510(4) .
