#------------------------------------------------------------------------------
#$Date: 2016-03-26 23:04:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180528 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/97/7219775.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_7219775
loop_
_publ_author_name
'Clegg, William'
'Holcroft, James M.'
'Martin, Nicola C.'
_publ_section_title
;
 Copper pyromellitates: a complex story
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2857
_journal_paper_doi               10.1039/C5CE00470E
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C10 H10 Cu2 O12,2 H2 O'
_chemical_formula_sum            'C10 H14 Cu2 O14'
_chemical_formula_weight         485.29
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.448(10)
_cell_angle_beta                 108.706(8)
_cell_angle_gamma                108.090(8)
_cell_formula_units_Z            1
_cell_length_a                   6.5120(10)
_cell_length_b                   6.9010(10)
_cell_length_c                   9.328(2)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10.0
_cell_volume                     368.51(12)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      240(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe-Siemens four-circle diffractometer'
_diffrn_measurement_method       'ω/θ scans with on-line profile fitting'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2592
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.002
_diffrn_reflns_theta_max         25.002
_diffrn_reflns_theta_min         2.361
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.968
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SHELXTL
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             244
_exptl_crystal_recrystallization_method
'Obtained direct from slow diffusion synthesis'
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1296
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0260
_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)+(0.0399P)²+0.4199P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1249
_reflns_number_total             1296
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00470e2.cif
_cod_data_source_block           kw25
_cod_depositor_comments
'Adding full bibliography for 7219775--7219784.cif.'
_cod_original_cell_volume        368.51(11)
_cod_database_code               7219775
#BEGIN Tags that were not found in dictionaries:
_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   0.307
_shelx_estimated_absorpt_t_max   0.890
#END Tags that were not found in dictionaries
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
Cu Cu 0.00502(5) 0.26574(4) 0.13393(3) 0.01161(17) Uani 1 1 d . .
C1 C 0.3626(4) 0.8823(4) 0.3489(3) 0.0104(5) Uani 1 1 d . .
C2 C 0.5903(4) 1.0185(4) 0.3827(3) 0.0100(5) Uani 1 1 d . .
C3 C 0.7242(4) 1.1352(4) 0.5326(3) 0.0117(5) Uani 1 1 d . .
H3 H 0.8762 1.2278 0.5544 0.014 Uiso 1 1 calc R U
C4 C 0.1982(4) 0.7654(4) 0.1868(3) 0.0114(5) Uani 1 1 d . .
C5 C 0.7089(4) 1.0327(4) 0.2664(3) 0.0117(5) Uani 1 1 d . .
O1 O 0.0371(3) 0.5999(3) 0.16939(19) 0.0146(4) Uani 1 1 d . .
O2 O 0.2297(3) 0.8515(3) 0.0761(2) 0.0165(4) Uani 1 1 d . .
O3 O 0.7477(3) 0.8788(3) 0.2199(2) 0.0198(4) Uani 1 1 d . .
O4 O 0.7741(3) 1.2106(3) 0.2321(2) 0.0148(4) Uani 1 1 d . .
O5 O 0.2489(3) 0.3179(3) 0.3382(2) 0.0181(4) Uani 1 1 d D .
H5A H 0.243(5) 0.361(5) 0.423(2) 0.027 Uiso 1 1 d D U
H5B H 0.382(3) 0.385(4) 0.342(3) 0.027 Uiso 1 1 d D U
O6 O 0.2657(4) 0.2776(4) 0.0646(2) 0.0295(5) Uani 1 1 d D .
H6A H 0.243(7) 0.287(6) -0.0265(19) 0.044 Uiso 1 1 d D U
H6B H 0.320(7) 0.184(5) 0.083(4) 0.044 Uiso 1 1 d D U
O7 O 0.6921(3) 0.5450(3) 0.3652(2) 0.0180(4) Uani 1 1 d D .
H7A H 0.723(6) 0.451(3) 0.324(3) 0.027 Uiso 1 1 d D U
H7B H 0.711(6) 0.643(3) 0.319(3) 0.027 Uiso 1 1 d D U
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
O1 Cu O2 102.39(7) . 2_565
O1 Cu O4 88.40(7) . 1_445
O1 Cu O5 91.22(7) . .
O1 Cu O6 101.58(9) . .
O2 Cu O4 93.62(8) 2_565 1_445
O2 Cu O5 166.19(8) 2_565 .
O2 Cu O6 93.15(8) 2_565 .
O4 Cu O5 89.02(8) 1_445 .
O4 Cu O6 166.45(9) 1_445 .
O5 Cu O6 81.70(8) . .
C2 C1 C3 119.0(2) . 2_676
C2 C1 C4 123.1(2) . .
C3 C1 C4 117.7(2) 2_676 .
C1 C2 C3 119.7(2) . .
C1 C2 C5 123.0(2) . .
C3 C2 C5 117.1(2) . .
C1 C3 C2 121.3(2) 2_676 .
C1 C3 H3 119.3 2_676 .
C2 C3 H3 119.3 . .
C1 C4 O1 119.0(2) . .
C1 C4 O2 116.5(2) . .
O1 C4 O2 124.4(2) . .
C2 C5 O3 118.7(2) . .
C2 C5 O4 116.0(2) . .
O3 C5 O4 125.2(2) . .
Cu O1 C4 132.93(16) . .
Cu O2 C4 119.01(16) 2_565 .
Cu O4 C5 117.99(16) 1_665 .
Cu O5 H5A 125(2) . .
Cu O5 H5B 113(2) . .
H5A O5 H5B 106.7(16) . .
Cu O6 H6A 116(3) . .
Cu O6 H6B 115(3) . .
H6A O6 H6B 108.9(17) . .
H7A O7 H7B 108.6(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O1 2.2319(17) .
Cu O2 1.9592(18) 2_565
Cu O4 1.9589(18) 1_445
Cu O5 1.9636(18) .
Cu O6 1.984(2) .
C1 C2 1.400(3) .
C1 C3 1.393(3) 2_676
C1 C4 1.509(3) .
C2 C3 1.390(3) .
C2 C5 1.514(3) .
C3 C1 1.393(3) 2_676
C3 H3 0.940 .
C4 O1 1.242(3) .
C4 O2 1.280(3) .
C5 O3 1.238(3) .
C5 O4 1.276(3) .
O2 Cu 1.9592(18) 2_565
O4 Cu 1.9590(18) 1_665
O5 H5A 0.837(10) .
O5 H5B 0.836(10) .
O6 H6A 0.827(10) .
O6 H6B 0.835(10) .
O7 H7A 0.829(10) .
O7 H7B 0.833(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O7 0.837(10) 1.884(14) 2.701(3) 165(3) 2_666
O5 H5B O7 0.836(10) 1.904(11) 2.739(3) 176(3) .
O6 H6A O1 0.827(10) 2.29(3) 2.827(3) 123(3) 2_565
O6 H6A O3 0.827(10) 2.07(3) 2.732(3) 137(3) 2_665
O6 H6B O2 0.835(10) 2.17(3) 2.891(3) 144(4) 1_545
O7 H7A O4 0.829(10) 1.966(10) 2.793(3) 175(3) 1_545
O7 H7B O3 0.833(10) 1.937(10) 2.768(3) 176(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C3 C1 C2 C3 -0.8(4) 2_676 .
C3 C1 C2 C5 173.7(2) 2_676 .
C4 C1 C2 C3 174.1(2) . .
C4 C1 C2 C5 -11.4(4) . .
C1 C2 C3 C1 0.8(4) . 2_676
C5 C2 C3 C1 -174.0(2) . 2_676
C2 C1 C4 O1 155.1(2) . .
C2 C1 C4 O2 -28.2(3) . .
C3 C1 C4 O1 -29.9(3) 2_676 .
C3 C1 C4 O2 146.8(2) 2_676 .
C1 C2 C5 O3 -64.6(3) . .
C1 C2 C5 O4 119.8(3) . .
C3 C2 C5 O3 110.1(3) . .
C3 C2 C5 O4 -65.6(3) . .
C1 C4 O1 Cu -92.2(2) . .
O2 C4 O1 Cu 91.3(3) . .
C1 C4 O2 Cu -170.09(16) . 2_565
O1 C4 O2 Cu 6.4(3) . 2_565
C2 C5 O4 Cu 162.22(16) . 1_665
O3 C5 O4 Cu -13.1(3) . 1_665
