#------------------------------------------------------------------------------
#$Date: 2017-06-29 04:43:14 +0300 (Thu, 29 Jun 2017) $
#$Revision: 198222 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/85/7228577.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_7228577
loop_
_publ_author_name
'Fidelli, Athena M.'
'Kessler, Vadim G.'
'Escuer, Albert'
'Papaefstathiou, Giannis S.'
_publ_section_title
;
 Cu(II) frameworks from a “mixed-ligand” approach
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01078H
_journal_year                    2017
_chemical_formula_sum            'C32 H24 Cu N4 O12'
_chemical_formula_weight         720.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                104.3800(10)
_cell_angle_beta                 106.1680(10)
_cell_angle_gamma                101.9190(10)
_cell_formula_units_Z            1
_cell_length_a                   7.9068(7)
_cell_length_b                   9.2354(9)
_cell_length_c                   11.0960(10)
_cell_measurement_reflns_used    3156
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.58
_cell_volume                     719.97(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type
'Bruker APEX-II CCD'_diffrn_measurement_method   'Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7126
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.385
_diffrn_reflns_theta_min         2.384
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             369
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.190
_exptl_transmission_factor_max   0.857
_exptl_transmission_factor_min   0.799
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3597
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0568P)²+0.2916P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3067
_reflns_number_total             3597
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce01078h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/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.

'_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        719.97(11)
_cod_database_code               7228577
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.799
_shelx_estimated_absorpt_t_max   0.857
_exptl_absorpt_special_details   'Bruker SADABS'
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.5000 0.5000 0.03401(12) Uani 1 2 d S . P
O1 O 0.5170(2) 0.47871(18) 0.28096(16) 0.0393(3) Uani 1 1 d D . .
O2 O 0.2718(2) 0.34965(18) 0.07852(15) 0.0423(4) Uani 1 1 d . . .
H2A H 0.2834 0.4286 0.0566 0.063 Uiso 1 1 calc R U .
O3 O 0.6584(3) 0.3811(2) 0.97166(19) 0.0598(5) Uani 1 1 d . . .
O4 O 0.4279(3) 0.2600(2) 0.78597(19) 0.0668(6) Uani 1 1 d . . .
O5 O 0.1959(3) 0.0095(2) 0.6696(2) 0.0823(8) Uani 1 1 d . . .
H5 H 0.2839 0.0892 0.7047 0.123 Uiso 1 1 calc R U .
O6 O 0.0887(2) -0.2003(2) 0.71043(17) 0.0523(4) Uani 1 1 d . . .
N1 N 0.2738(2) 0.54449(19) 0.40523(17) 0.0347(4) Uani 1 1 d . . .
N2 N 0.3760(2) 0.2733(2) 0.38652(18) 0.0372(4) Uani 1 1 d . . .
C1 C 0.1794(3) 0.6210(3) 0.4649(2) 0.0425(5) Uani 1 1 d . . .
H1 H 0.2209 0.6584 0.5571 0.051 Uiso 1 1 calc R U .
C2 C 0.0200(3) 0.6469(3) 0.3935(3) 0.0481(5) Uani 1 1 d . . .
H2 H -0.0431 0.7030 0.4369 0.058 Uiso 1 1 calc R U .
C3 C -0.0420(3) 0.5875(3) 0.2574(3) 0.0472(5) Uani 1 1 d . . .
H3 H -0.1488 0.6023 0.2074 0.057 Uiso 1 1 calc R U .
C4 C 0.0541(3) 0.5063(3) 0.1955(2) 0.0390(5) Uani 1 1 d . . .
H4 H 0.0130 0.4654 0.1034 0.047 Uiso 1 1 calc R U .
C5 C 0.2120(3) 0.4862(2) 0.2715(2) 0.0322(4) Uani 1 1 d . . .
C6 C 0.3271(3) 0.3918(2) 0.2146(2) 0.0339(4) Uani 1 1 d . . .
C7 C 0.3052(3) 0.2455(2) 0.2553(2) 0.0341(4) Uani 1 1 d . . .
C8 C 0.2147(3) 0.0969(3) 0.1665(2) 0.0424(5) Uani 1 1 d . . .
H8 H 0.1672 0.0806 0.0759 0.051 Uiso 1 1 calc R U .
C9 C 0.1962(4) -0.0272(3) 0.2149(3) 0.0542(6) Uani 1 1 d . . .
H9 H 0.1358 -0.1287 0.1571 0.065 Uiso 1 1 calc R U .
C10 C 0.2677(4) 0.0005(3) 0.3493(3) 0.0566(7) Uani 1 1 d . . .
H10 H 0.2553 -0.0818 0.3836 0.068 Uiso 1 1 calc R U .
C11 C 0.3577(4) 0.1517(3) 0.4320(3) 0.0497(6) Uani 1 1 d . . .
H11 H 0.4076 0.1702 0.5228 0.060 Uiso 1 1 calc R U .
C12 C 0.5019(3) 0.1215(2) 0.9426(2) 0.0311(4) Uani 1 1 d . . .
C13 C 0.3647(3) -0.0239(2) 0.87643(19) 0.0314(4) Uani 1 1 d . . .
C14 C 0.3696(3) -0.1392(2) 0.9363(2) 0.0331(4) Uani 1 1 d . . .
H14 H 0.2798 -0.2356 0.8918 0.040 Uiso 1 1 calc R U .
C15 C 0.5311(3) 0.2655(2) 0.8986(2) 0.0368(4) Uani 1 1 d . . .
C16 C 0.2053(3) -0.0770(3) 0.7445(2) 0.0403(5) Uani 1 1 d . . .
H1A H 0.542(5) 0.560(3) 0.271(3) 0.075(10) 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'
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'
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
N1 Cu1 N1 180.00(9) . 2_666
N1 Cu1 N2 87.21(7) . .
N1 Cu1 N2 92.79(7) 2_666 .
N1 Cu1 N2 92.79(7) . 2_666
N1 Cu1 N2 87.21(7) 2_666 2_666
N2 Cu1 N2 180.0 . 2_666
N1 Cu1 O1 104.09(6) . 2_666
N1 Cu1 O1 75.91(6) 2_666 2_666
N2 Cu1 O1 106.75(6) . 2_666
N2 Cu1 O1 73.25(6) 2_666 2_666
N1 Cu1 O1 75.91(6) . .
N1 Cu1 O1 104.09(6) 2_666 .
N2 Cu1 O1 73.25(6) . .
N2 Cu1 O1 106.75(6) 2_666 .
O1 Cu1 O1 180.0 2_666 .
C6 O1 Cu1 93.26(11) . .
C1 N1 C5 119.45(18) . .
C1 N1 Cu1 124.28(15) . .
C5 N1 Cu1 116.22(14) . .
C11 N2 C7 118.5(2) . .
C11 N2 Cu1 125.36(17) . .
C7 N2 Cu1 116.17(13) . .
N1 C1 C2 121.9(2) . .
C3 C2 C1 118.3(2) . .
C4 C3 C2 119.9(2) . .
C3 C4 C5 119.1(2) . .
N1 C5 C4 121.3(2) . .
N1 C5 C6 114.45(17) . .
C4 C5 C6 124.15(19) . .
O2 C6 O1 113.85(17) . .
O2 C6 C7 109.47(16) . .
O1 C6 C7 105.00(15) . .
O2 C6 C5 112.43(16) . .
O1 C6 C5 108.21(16) . .
C7 C6 C5 107.45(16) . .
N2 C7 C8 122.39(19) . .
N2 C7 C6 114.25(17) . .
C8 C7 C6 123.32(19) . .
C7 C8 C9 118.5(2) . .
C10 C9 C8 119.5(2) . .
C11 C10 C9 118.8(2) . .
N2 C11 C10 122.3(2) . .
C14 C12 C13 117.36(17) 2_657 .
C14 C12 C15 114.11(18) 2_657 .
C13 C12 C15 128.53(18) . .
C14 C13 C12 117.67(18) . .
C14 C13 C16 113.01(18) . .
C12 C13 C16 129.32(17) . .
C12 C14 C13 124.97(19) 2_657 .
O3 C15 O4 122.08(19) . .
O3 C15 C12 118.18(19) . .
O4 C15 C12 119.69(19) . .
O6 C16 O5 120.0(2) . .
O6 C16 C13 119.85(19) . .
O5 C16 C13 120.15(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.9860(17) .
Cu1 N1 1.9861(17) 2_666
Cu1 N2 2.0209(18) .
Cu1 N2 2.0209(18) 2_666
Cu1 O1 2.4329(16) 2_666
Cu1 O1 2.4329(16) .
O1 C6 1.426(3) .
O2 C6 1.376(2) .
O3 C15 1.217(3) .
O4 C15 1.271(3) .
O5 C16 1.286(3) .
O6 C16 1.204(3) .
N1 C1 1.324(3) .
N1 C5 1.350(3) .
N2 C11 1.339(3) .
N2 C7 1.342(3) .
C1 C2 1.391(3) .
C2 C3 1.374(4) .
C3 C4 1.371(3) .
C4 C5 1.375(3) .
C5 C6 1.536(3) .
C6 C7 1.520(3) .
C7 C8 1.377(3) .
C8 C9 1.380(3) .
C9 C10 1.375(4) .
C10 C11 1.374(4) .
C12 C14 1.388(3) 2_657
C12 C13 1.409(3) .
C12 C15 1.522(3) .
C13 C14 1.389(3) .
C13 C16 1.528(3) .
C14 C12 1.388(3) 2_657
