#------------------------------------------------------------------------------
#$Date: 2016-03-26 23:04:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180528 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/97/7219776.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_7219776
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 H14 Cu2 O14,4 H2 O'
_chemical_formula_sum            'C10 H22 Cu2 O18'
_chemical_formula_weight         557.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 113.503(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1518(8)
_cell_length_b                   18.1413(11)
_cell_length_c                   9.5816(6)
_cell_measurement_reflns_used    6591
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.133
_cell_measurement_theta_min      2.318
_cell_volume                     1937.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      160(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'narrow-frame ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.179
_diffrn_reflns_theta_min         2.145
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.287
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1136
_exptl_crystal_recrystallization_method
'Obtained direct from slow diffusion synthesis'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2253
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0285P)²+2.8396P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2063
_reflns_number_total             2253
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce00470e2.cif
_cod_data_source_block           wc57
_cod_depositor_comments
'Adding full bibliography for 7219775--7219784.cif.'
_cod_database_code               7219776
#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   0.645
_shelx_estimated_absorpt_t_max   0.658
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Cu Cu 0.22001(2) 0.55931(2) 0.33081(2) 0.01032(8) Uani 1 1 d . .
C1 C 0.44016(15) 0.71960(9) 0.24300(19) 0.0112(3) Uani 1 1 d . .
C2 C 0.38191(15) 0.78628(9) 0.23552(19) 0.0113(3) Uani 1 1 d . .
H2 H 0.3011 0.7862 0.2261 0.014 Uiso 1 1 calc R U
C3 C 0.43980(14) 0.85345(9) 0.24163(18) 0.0098(3) Uani 1 1 d . .
C4 C 0.37234(15) 0.64845(9) 0.2286(2) 0.0131(3) Uani 1 1 d . .
C5 C 0.36641(15) 0.92225(9) 0.22504(19) 0.0097(3) Uani 1 1 d . .
O1 O 0.37017(13) 0.60314(7) 0.13036(17) 0.0231(3) Uani 1 1 d . .
O2 O 0.32068(12) 0.64135(7) 0.32001(15) 0.0164(3) Uani 1 1 d . .
O3 O 0.29707(11) 0.92515(7) 0.29231(15) 0.0145(3) Uani 1 1 d . .
O4 O 0.37426(11) 0.97418(6) 0.13968(14) 0.0114(2) Uani 1 1 d . .
O5 O 0.34838(12) 0.53638(7) 0.52782(16) 0.0179(3) Uani 1 1 d D .
H5A H 0.3523(19) 0.4945(7) 0.564(3) 0.027 Uiso 1 1 d D U
H5B H 0.4162(12) 0.5547(11) 0.557(3) 0.027 Uiso 1 1 d D U
O6 O 0.10433(12) 0.57889(8) 0.12393(15) 0.0181(3) Uani 1 1 d D .
H6A H 0.1067(19) 0.5594(12) 0.0470(19) 0.027 Uiso 1 1 d D U
H6B H 0.0341(11) 0.5906(14) 0.107(2) 0.027 Uiso 1 1 d D U
O7 O 0.11551(12) 0.63051(7) 0.42583(14) 0.0145(3) Uani 1 1 d D .
H7A H 0.1516(19) 0.6223(11) 0.5185(12) 0.022 Uiso 1 1 d D U
H7B H 0.114(2) 0.6766(6) 0.414(2) 0.022 Uiso 1 1 d D U
O8 O 0.55669(13) 0.61173(9) 0.61276(18) 0.0244(3) Uani 1 1 d D .
H8A H 0.6191(15) 0.5988(15) 0.6851(18) 0.037 Uiso 1 1 d D U
H8B H 0.571(2) 0.6158(16) 0.5353(17) 0.037 Uiso 1 1 d D U
O9 O 0.12325(18) 0.77701(9) 0.4006(2) 0.0422(5) Uani 1 1 d D .
H9A H 0.156(2) 0.7936(17) 0.4900(16) 0.063 Uiso 1 1 d D U
H9B H 0.0594(18) 0.8007(17) 0.358(3) 0.063 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
O2 Cu O4 175.22(5) . 4_545
O2 Cu O5 86.44(6) . .
O2 Cu O6 91.15(6) . .
O2 Cu O7 92.90(5) . .
O4 Cu O5 88.90(5) 4_545 .
O4 Cu O6 93.60(6) 4_545 .
O4 Cu O7 86.48(5) 4_545 .
O5 Cu O6 173.57(6) . .
O5 Cu O7 95.36(5) . .
O6 Cu O7 90.71(5) . .
C1 C1 C2 119.43(10) 2_655 .
C1 C1 C4 121.03(9) 2_655 .
C2 C1 C4 119.48(15) . .
C1 C2 H2 119.3 . .
C1 C2 C3 121.33(15) . .
H2 C2 C3 119.3 . .
C2 C3 C3 119.23(10) . 2_655
C2 C3 C5 116.86(14) . .
C3 C3 C5 123.88(9) 2_655 .
C1 C4 O1 118.78(16) . .
C1 C4 O2 115.20(15) . .
O1 C4 O2 126.01(16) . .
C3 C5 O3 118.26(15) . .
C3 C5 O4 119.16(15) . .
O3 C5 O4 122.54(15) . .
Cu O2 C4 127.22(12) . .
Cu O4 C5 106.55(10) 4 .
Cu O5 H5A 119.3(15) . .
Cu O5 H5B 123.0(16) . .
H5A O5 H5B 110.1(15) . .
Cu O6 H6A 124.0(16) . .
Cu O6 H6B 121.2(16) . .
H6A O6 H6B 109.2(15) . .
Cu O7 H7A 100.8(16) . .
Cu O7 H7B 120.2(16) . .
H7A O7 H7B 107.1(14) . .
H8A O8 H8B 108.6(15) . .
H9A O9 H9B 106.7(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu O2 1.9553(12) .
Cu O4 2.0090(12) 4_545
Cu O5 1.9548(13) .
Cu O6 1.9517(13) .
Cu O7 2.2432(13) .
C1 C1 1.406(3) 2_655
C1 C2 1.389(2) .
C1 C4 1.508(2) .
C2 H2 0.950 .
C2 C3 1.397(2) .
C3 C3 1.407(3) 2_655
C3 C5 1.505(2) .
C4 O1 1.242(2) .
C4 O2 1.271(2) .
C5 O3 1.250(2) .
C5 O4 1.276(2) .
O4 Cu 2.0090(12) 4
O5 H5A 0.828(9) .
O5 H5B 0.827(9) .
O6 H6A 0.828(9) .
O6 H6B 0.829(9) .
O7 H7A 0.832(9) .
O7 H7B 0.843(9) .
O8 H8A 0.832(10) .
O8 H8B 0.832(9) .
O9 H9A 0.843(10) .
O9 H9B 0.838(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 O1 0.828(9) 1.866(10) 2.6897(19) 173(2) 6_566
O5 H5B O8 0.827(9) 1.883(9) 2.701(2) 170(2) .
O6 H6A O4 0.828(9) 1.989(10) 2.8103(18) 172(2) 7_565
O6 H6B O7 0.829(9) 1.865(10) 2.6880(19) 172(3) 2
O7 H7A O3 0.832(9) 1.874(10) 2.6746(18) 161(2) 7_566
O7 H7B O9 0.843(9) 1.833(10) 2.674(2) 175(2) .
O8 H8A O3 0.832(10) 2.037(14) 2.816(2) 156(2) 8_566
O8 H8B O1 0.832(9) 1.995(12) 2.809(2) 166(3) 2_655
O9 H9A O2 0.843(10) 2.093(15) 2.893(2) 158(3) 7_566
O9 H9B O8 0.838(10) 2.22(2) 2.941(2) 145(2) 7_566
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
C1 C1 C2 C3 0.0(3) 2_655 .
C4 C1 C2 C3 -177.16(16) . .
C1 C2 C3 C3 -1.1(3) . 2_655
C1 C2 C3 C5 177.16(15) . .
C1 C1 C4 O1 -51.5(3) 2_655 .
C1 C1 C4 O2 129.3(2) 2_655 .
C2 C1 C4 O1 125.59(19) . .
C2 C1 C4 O2 -53.6(2) . .
C2 C3 C5 O3 41.6(2) . .
C2 C3 C5 O4 -136.21(17) . .
C3 C3 C5 O3 -140.2(2) 2_655 .
C3 C3 C5 O4 42.0(3) 2_655 .
C1 C4 O2 Cu 177.49(11) . .
O1 C4 O2 Cu -1.6(3) . .
C3 C5 O4 Cu -173.10(12) . 4
O3 C5 O4 Cu 9.19(19) . 4
