data_Cu(HhpOa)
_audit_creation_date               2019-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2014/7'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C16 H18 Cu O10, 2(H2 O)'
_chemical_formula_sum              'C16 H22 Cu O12'
_chemical_formula_weight           469.87
_chemical_melting_point            ?
_chemical_oxdiff_formula           'Cu1 c9 o3 H6'
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'

_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.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/n 1'
_space_group_name_Hall             '-P 2yn'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                     7.1067(3)
_cell_length_b                     7.0650(3)
_cell_length_c                     19.0913(7)
_cell_angle_alpha                  90
_cell_angle_beta                   90.077(3)
_cell_angle_gamma                  90
_cell_volume                       958.55(7)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      2825
_cell_measurement_temperature      130.01(10)
_cell_measurement_theta_max        73.6020
_cell_measurement_theta_min        6.6280
_shelx_estimated_absorpt_T_max     0.856
_shelx_estimated_absorpt_T_min     0.568
_exptl_absorpt_coefficient_mu      2.206
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.59960
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light blue'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      blue
_exptl_crystal_density_diffrn      1.628
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         'rect. Prism'
_exptl_crystal_F_000               486
_exptl_crystal_size_max            0.289
_exptl_crystal_size_mid            0.096
_exptl_crystal_size_min            0.073
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0582
_diffrn_reflns_av_unetI/netI       0.0460
_diffrn_reflns_Laue_measured_fraction_full  0.995
_diffrn_reflns_Laue_measured_fraction_max  0.975
_diffrn_reflns_limit_h_max         8
_diffrn_reflns_limit_h_min         -8
_diffrn_reflns_limit_k_max         8
_diffrn_reflns_limit_k_min         -8
_diffrn_reflns_limit_l_max         10
_diffrn_reflns_limit_l_min         -23
_diffrn_reflns_number              5779
_diffrn_reflns_point_group_measured_fraction_full  0.995
_diffrn_reflns_point_group_measured_fraction_max  0.975
_diffrn_reflns_theta_full          67.684
_diffrn_reflns_theta_max           74.550
_diffrn_reflns_theta_min           4.632
_diffrn_ambient_temperature        130.01(10)
_diffrn_detector_area_resol_mean   10.2273
_diffrn_measured_fraction_theta_full  0.995
_diffrn_measured_fraction_theta_max  0.975
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -122.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8092    0.0000  120.0000 171

#__ type_ start__ end____ width___ exp.time_
  2 omega  -46.00  -16.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8092   37.0000 -180.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega   32.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8092 -125.0000  -60.0000 57

#__ type_ start__ end____ width___ exp.time_
  4 omega   33.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8092 -125.0000  120.0000 49

#__ type_ start__ end____ width___ exp.time_
  5 omega -130.00 -104.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -111.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
  6 omega -139.00 -113.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -111.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega  101.00  155.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  111.0000  150.0000 54

#__ type_ start__ end____ width___ exp.time_
  8 omega   45.00  108.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -94.0000 -180.0000 63

#__ type_ start__ end____ width___ exp.time_
  9 omega   63.00   90.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -45.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
 10 omega   37.00   69.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -77.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
 11 omega  107.00  133.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 12 omega   31.00   86.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000   30.0000 55

#__ type_ start__ end____ width___ exp.time_
 13 omega  148.00  177.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  111.0000 -180.0000 29

#__ type_ start__ end____ width___ exp.time_
 14 omega   27.00  145.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -20.0000 -160.0000 118

#__ type_ start__ end____ width___ exp.time_
 15 omega   31.00   89.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000  120.0000 58

#__ type_ start__ end____ width___ exp.time_
 16 omega  101.00  164.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  111.0000    0.0000 63

#__ type_ start__ end____ width___ exp.time_
 17 omega  122.00  148.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  178.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 18 omega   66.00   91.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 19 omega   63.00  106.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -94.0000   90.0000 43

#__ type_ start__ end____ width___ exp.time_
 20 omega   50.00   91.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393  -30.0000  -30.0000 41

#__ type_ start__ end____ width___ exp.time_
 21 omega   42.00   94.00   1.0000   23.0000
omega____ theta____ kappa____ phi______ frames
    -      107.9393 -111.0000    0.0000 52
;
_diffrn_measurement_device_type    'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_UB_11        -0.1524112000
_diffrn_orient_matrix_UB_12        0.1540574000
_diffrn_orient_matrix_UB_13        0.0061702000
_diffrn_orient_matrix_UB_21        0.1454350000
_diffrn_orient_matrix_UB_22        0.1517396000
_diffrn_orient_matrix_UB_23        -0.0206574000
_diffrn_orient_matrix_UB_31        -0.0511097000
_diffrn_orient_matrix_UB_32        -0.0280937000
_diffrn_orient_matrix_UB_33        -0.0777602000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  1704
_reflns_number_total               1905
_reflns_odcompleteness_completeness  99.37
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       67.62
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution      'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max           0.824
_refine_diff_density_min           -0.825
_refine_diff_density_rms           0.118
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.073
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       149
_refine_ls_number_reflns           1905
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0491
_refine_ls_R_factor_gt             0.0451
_refine_ls_restrained_S_all        1.073
_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)+(0.0899P)²+0.2336P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1274
_refine_ls_wR_factor_ref           0.1337
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Free rotating group:
 H5A(H5B), O1S(H1SA,H1SB)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C4(H4A), C5(H5)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     ?
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
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Cu1 Cu 0.5000 0.5000 0.5000 0.0148(2) Uani 1 2 d S T P . .
 O1 O 0.7254(2) 0.6293(2) 0.47176(7) 0.0176(3) Uani 1 1 d . . . . .
 O2 O 1.0063(2) 0.7527(2) 0.48773(8) 0.0188(4) Uani 1 1 d . . . . .
 O3 O 0.6730(2) 0.5621(2) 0.60635(7) 0.0185(3) Uani 1 1 d . . . . .
 O5 O 0.6276(2) 0.2528(2) 0.49210(8) 0.0202(4) Uani 1 1 d . . . . .
 H5A H 0.5849 0.1781 0.4564 0.030 Uiso 1 1 d . . . . .
 H5B H 0.7488 0.2642 0.4899 0.049(11) Uiso 1 1 d G . . . .
 O4 O 0.3678(2) 0.5570(3) 0.87315(8) 0.0233(4) Uani 1 1 d . . . . .
 H4 H 0.4337 0.6129 0.9017 0.035 Uiso 1 1 calc GR . . . .
 O1S O 0.4926(3) 0.0031(2) 0.40254(10) 0.0248(4) Uani 1 1 d . . . . .
 H1SA H 0.5954 -0.0376 0.3855 0.037 Uiso 1 1 d G . . . .
 H1SB H 0.4517 -0.0882 0.4272 0.042(10) Uiso 1 1 d G . . . .
 C1 C 0.8595(3) 0.6810(3) 0.51112(10) 0.0156(4) Uani 1 1 d . . . . .
 C3 C 0.6058(3) 0.5710(3) 0.67504(10) 0.0161(4) Uani 1 1 d . . . . .
 C2 C 0.8399(3) 0.6651(3) 0.59040(10) 0.0175(4) Uani 1 1 d . . . . .
 H2A H 0.9485 0.6004 0.6098 0.021 Uiso 1 1 calc R . . . .
 H2B H 0.8334 0.7904 0.6110 0.024(7) Uiso 1 1 calc R . . . .
 C8 C 0.6982(3) 0.6608(3) 0.72926(11) 0.0199(5) Uani 1 1 d . . . . .
 H8 H 0.8120 0.7222 0.7214 0.029(8) Uiso 1 1 calc R . . . .
 C6 C 0.4501(3) 0.5668(3) 0.80799(10) 0.0174(4) Uani 1 1 d . . . . .
 C7 C 0.6182(3) 0.6583(3) 0.79645(11) 0.0195(5) Uani 1 1 d . . . . .
 H7 H 0.6791 0.7188 0.8333 0.024(7) Uiso 1 1 calc R . . . .
 C4 C 0.4356(3) 0.4795(3) 0.68605(12) 0.0189(5) Uani 1 1 d . . . . .
 H4A H 0.3743 0.4201 0.6490 0.018(6) Uiso 1 1 calc R . . . .
 C5 C 0.3570(3) 0.4773(3) 0.75293(12) 0.0196(5) Uani 1 1 d . . . . .
 H5 H 0.2429 0.4163 0.7607 0.024 Uiso 1 1 calc R . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Cu1 O1 1.9220(14) . ?
 Cu1 O1 1.9221(14) 3_666 ?
 Cu1 O3 2.4124(14) 3_666 ?
 Cu1 O3 2.4124(14) . ?
 Cu1 O5 1.9741(16) . ?
 Cu1 O5 1.9741(16) 3_666 ?
 O1 C1 1.267(3) . ?
 O2 C1 1.243(3) . ?
 O3 C3 1.398(2) . ?
 O3 C2 1.425(3) . ?
 O5 H5A 0.91(3) . ?
 O5 H5B 0.8658 . ?
 O4 H4 0.8200 . ?
 O4 C6 1.377(2) . ?
 O1S H1SA 0.8498 . ?
 O1S H1SB 0.8499 . ?
 C1 C2 1.524(3) . ?
 C3 C8 1.380(3) . ?
 C3 C4 1.388(3) . ?
 C2 H2A 0.9700 . ?
 C2 H2B 0.9700 . ?
 C8 H8 0.9300 . ?
 C8 C7 1.404(3) . ?
 C6 C7 1.377(3) . ?
 C6 C5 1.394(3) . ?
 C7 H7 0.9300 . ?
 C4 H4A 0.9300 . ?
 C4 C5 1.394(3) . ?
 C5 H5 0.9300 . ?

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
  _geom_angle_publ_flag
 O1 Cu1 O1 180.0 . 3_666 ?
 O1 Cu1 O3 74.08(5) 3_666 3_666 ?
 O1 Cu1 O3 105.92(5) 3_666 . ?
 O1 Cu1 O3 105.92(5) . 3_666 ?
 O1 Cu1 O3 74.08(5) . . ?
 O1 Cu1 O5 89.09(7) . 3_666 ?
 O1 Cu1 O5 89.09(7) 3_666 . ?
 O1 Cu1 O5 90.91(7) 3_666 3_666 ?
 O1 Cu1 O5 90.91(7) . . ?
 O3 Cu1 O3 180.0 . 3_666 ?
 O5 Cu1 O3 90.49(6) 3_666 . ?
 O5 Cu1 O3 89.51(6) 3_666 3_666 ?
 O5 Cu1 O3 90.49(6) . 3_666 ?
 O5 Cu1 O3 89.51(6) . . ?
 O5 Cu1 O5 180.00(8) 3_666 . ?
 C1 O1 Cu1 126.69(13) . . ?
 C3 O3 Cu1 128.59(13) . . ?
 C3 O3 C2 117.57(16) . . ?
 C2 O3 Cu1 109.66(11) . . ?
 Cu1 O5 H5A 115(2) . . ?
 Cu1 O5 H5B 112.2 . . ?
 H5A O5 H5B 110.3 . . ?
 C6 O4 H4 109.5 . . ?
 H1SA O1S H1SB 104.5 . . ?
 O1 C1 C2 119.86(17) . . ?
 O2 C1 O1 122.37(18) . . ?
 O2 C1 C2 117.70(17) . . ?
 C8 C3 O3 124.20(19) . . ?
 C8 C3 C4 120.98(19) . . ?
 C4 C3 O3 114.82(18) . . ?
 O3 C2 C1 109.11(15) . . ?
 O3 C2 H2A 109.9 . . ?
 O3 C2 H2B 109.9 . . ?
 C1 C2 H2A 109.9 . . ?
 C1 C2 H2B 109.9 . . ?
 H2A C2 H2B 108.3 . . ?
 C3 C8 H8 120.4 . . ?
 C3 C8 C7 119.1(2) . . ?
 C7 C8 H8 120.4 . . ?
 O4 C6 C5 117.2(2) . . ?
 C7 C6 O4 122.57(19) . . ?
 C7 C6 C5 120.27(19) . . ?
 C8 C7 H7 119.8 . . ?
 C6 C7 C8 120.32(19) . . ?
 C6 C7 H7 119.8 . . ?
 C3 C4 H4A 120.2 . . ?
 C3 C4 C5 119.6(2) . . ?
 C5 C4 H4A 120.2 . . ?
 C6 C5 C4 119.7(2) . . ?
 C6 C5 H5 120.2 . . ?
 C4 C5 H5 120.2 . . ?

_olex2_date_sample_data_collection  2014-08-26
_olex2_submission_special_instructions  'No special instructions were received'
