data_cu_tca_nh4_1_0m_a_sq
_audit_creation_date               2023-11-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number       '2018/3'
_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          
 '2(C21 H12 N O6), 2(C21 H15 N O6), 6(H4 N), 1.5(H2 O2), 0.875[C3H7NO]'
_chemical_formula_sum              'C86.62 H87.12 N10.88 O27.88'
_chemical_formula_weight           1726.63
_chemical_absolute_configuration   ?
_chemical_melting_point            ?
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'
 'N' 'N' 0.0311 0.0180 '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        'cubic'
_space_group_IT_number             197
_space_group_name_H-M_alt          'I 2 3'
_space_group_name_Hall             'I 2 2 3'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-x, y, -z'
 'x, -y, -z'
 'z, x, y'
 'z, -x, -y'
 '-z, -x, y'
 '-z, x, -y'
 'y, z, x'
 '-y, z, -x'
 'y, -z, -x'
 '-y, -z, x'
 'x+1/2, y+1/2, z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z+1/2'
 'z+1/2, x+1/2, y+1/2'
 'z+1/2, -x+1/2, -y+1/2'
 '-z+1/2, -x+1/2, y+1/2'
 '-z+1/2, x+1/2, -y+1/2'
 'y+1/2, z+1/2, x+1/2'
 '-y+1/2, z+1/2, -x+1/2'
 'y+1/2, -z+1/2, -x+1/2'
 '-y+1/2, -z+1/2, x+1/2'

_cell_length_a                     20.9737(2)
_cell_length_b                     20.9737(2)
_cell_length_c                     20.9737(2)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       9226.2(3)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      5714
_cell_measurement_temperature      170.00
_cell_measurement_theta_max        65.21
_cell_measurement_theta_min        5.17
_shelx_estimated_absorpt_T_max     0.821
_shelx_estimated_absorpt_T_min     0.770
_exptl_absorpt_coefficient_mu      0.789
_exptl_absorpt_correction_T_max    0.7528
_exptl_absorpt_correction_T_min    0.6023
_exptl_absorpt_correction_type     none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1249 before and 0.0829 after correction.
The Ratio of minimum to maximum transmission is 0.8001.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      1.243
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               3624
_exptl_crystal_size_max            0.35
_exptl_crystal_size_mid            0.3
_exptl_crystal_size_min            0.26
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1528
_diffrn_reflns_av_unetI/netI       0.0642
_diffrn_reflns_Laue_measured_fraction_full  0.997
_diffrn_reflns_Laue_measured_fraction_max  0.997
_diffrn_reflns_limit_h_max         16
_diffrn_reflns_limit_h_min         -23
_diffrn_reflns_limit_k_max         24
_diffrn_reflns_limit_k_min         -22
_diffrn_reflns_limit_l_max         24
_diffrn_reflns_limit_l_min         -20
_diffrn_reflns_number              21578
_diffrn_reflns_point_group_measured_fraction_full  0.998
_diffrn_reflns_point_group_measured_fraction_max  0.998
_diffrn_reflns_theta_full          66.444
_diffrn_reflns_theta_max           66.444
_diffrn_reflns_theta_min           5.165
_diffrn_ambient_temperature        170.00
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.997
_diffrn_measured_fraction_theta_max  0.997
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54178
_diffrn_source                     ?
_diffrn_source_current             1.2
_diffrn_source_power               0.06
_diffrn_source_voltage             50.0
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.838
_reflns_Friedel_fraction_full      0.999
_reflns_Friedel_fraction_max       0.999
_reflns_number_gt                  2004
_reflns_number_total               2724
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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         'SAINT V8.40B (?, 2016)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics      'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max           0.245
_refine_diff_density_min           -0.312
_refine_diff_density_rms           0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 704 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     0.2(2)
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.019
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       184
_refine_ls_number_reflns           2724
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0932
_refine_ls_R_factor_gt             0.0745
_refine_ls_restrained_S_all        1.019
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.1564P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.2108
_refine_ls_wR_factor_ref           0.2270
_refine_special_details            ?
_olex2_refinement_description
;
1. Others
 Fixed Sof: H00M(0.5)
2.a Riding coordinates:
 N006(H00A), N006(H00C,H00F,H00H), O00M(H00M)
2.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00D(H00D), C00E(H00E), C00G(H00G), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L)
2.c Idealised tetrahedral OH refined as rotating group:
 O002(H002)
;
_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
 O001 O 0.7302(2) 0.3938(2) 0.0206(2) 0.0779(12) Uani 1 1 d . . . . .
 O002 O 0.7317(2) 0.4802(2) 0.1011(2) 0.0800(13) Uani 1 1 d . . . . .
 H002 H 0.727507 0.451716 0.073277 0.120 Uiso 1 1 calc R U . . .
 O003 O 0.8333(2) 0.4143(2) 0.0134(2) 0.0874(14) Uani 1 1 d . . . . .
 O004 O 0.6266(3) 0.4885(3) 0.0877(3) 0.105(2) Uani 1 1 d . . . . .
 N005 N 0.6747(5) 0.6747(5) 0.3253(5) 0.102(4) Uani 1 3 d S T P . .
 N006 N 0.8869(3) 0.5038(3) 0.0920(3) 0.0823(15) Uani 1 1 d . . . . .
 H00A H 0.905490 0.534953 0.068246 0.099 Uiso 1 1 d R U . . .
 H00C H 0.869240 0.474123 0.065776 0.099 Uiso 1 1 d R U . . .
 H00F H 0.916890 0.484903 0.117076 0.099 Uiso 1 1 d R U . . .
 H00H H 0.856040 0.521173 0.117076 0.099 Uiso 1 1 d R U . . .
 C007 C 0.7858(3) 0.3837(3) -0.0019(3) 0.0696(14) Uani 1 1 d . . . . .
 C008 C 0.6762(3) 0.5025(3) 0.1163(3) 0.0738(14) Uani 1 1 d . . . . .
 C009 C 0.7928(3) 0.3311(3) -0.0501(3) 0.0644(13) Uani 1 1 d . . . . .
 C00A C 0.6761(3) 0.5477(3) 0.1703(3) 0.0711(14) Uani 1 1 d . . . . .
 C00B C 0.7330(3) 0.5701(3) 0.1945(3) 0.0788(17) Uani 1 1 d . . . . .
 H00B H 0.772061 0.556642 0.175983 0.095 Uiso 1 1 calc R U . . .
 C00C C 0.6762(3) 0.6324(3) 0.2726(3) 0.084(2) Uani 1 1 d . . . . .
 C00D C 0.7401(3) 0.3043(3) -0.0774(3) 0.0746(16) Uani 1 1 d . . . . .
 H00D H 0.698895 0.318599 -0.065243 0.090 Uiso 1 1 calc R U . . .
 C00E C 0.7460(3) 0.2563(4) -0.1230(3) 0.083(2) Uani 1 1 d . . . . .
 H00E H 0.709231 0.238697 -0.142741 0.100 Uiso 1 1 calc R U . . .
 N00F N 0.8139(4) 0.1861(4) -0.1861(4) 0.100(4) Uani 1 3 d S T P . .
 C00G C 0.7336(3) 0.6123(3) 0.2459(4) 0.087(2) Uani 1 1 d . . . . .
 H00G H 0.772972 0.627205 0.262680 0.104 Uiso 1 1 calc R U . . .
 C00H C 0.8069(3) 0.2343(3) -0.1392(3) 0.0806(19) Uani 1 1 d . . . . .
 C00I C 0.8527(3) 0.3094(3) -0.0656(3) 0.085(2) Uani 1 1 d . . . . .
 H00I H 0.889099 0.327973 -0.046133 0.102 Uiso 1 1 calc R U . . .
 C00J C 0.6198(4) 0.6107(5) 0.2466(4) 0.109(3) Uani 1 1 d . . . . .
 H00J H 0.580370 0.624921 0.263812 0.130 Uiso 1 1 calc R U . . .
 C00K C 0.8603(3) 0.2606(4) -0.1095(4) 0.096(3) Uani 1 1 d . . . . .
 H00K H 0.901751 0.245190 -0.119334 0.116 Uiso 1 1 calc R U . . .
 C00L C 0.6197(4) 0.5691(4) 0.1964(4) 0.097(3) Uani 1 1 d . . . . .
 H00L H 0.580305 0.554701 0.179263 0.117 Uiso 1 1 calc R U . . .
 O00M O 0.500000 0.500000 0.0547(9) 0.207(7) Uani 1 2 d S T P . .
 H00M H 0.538870 0.513740 0.059256 0.310 Uiso 0.5 1 d R U P . .


_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
 O001 C007 1.274(8) . ?
 O002 H002 0.8400 . ?
 O002 C008 1.294(8) . ?
 O003 C007 1.230(8) . ?
 O004 C008 1.237(8) . ?
 N005 C00C 1.417(5) 11_566 ?
 N005 C00C 1.417(5) 8_656 ?
 N005 C00C 1.418(5) . ?
 N006 H00A 0.9099 . ?
 N006 H00C 0.9102 . ?
 N006 H00F 0.9100 . ?
 N006 H00H 0.9097 . ?
 C007 C009 1.503(6) . ?
 C008 C00A 1.479(7) . ?
 C009 C00D 1.367(8) . ?
 C009 C00I 1.375(9) . ?
 C00A C00B 1.379(8) . ?
 C00A C00L 1.377(9) . ?
 C00B H00B 0.9500 . ?
 C00B C00G 1.396(8) . ?
 C00C C00G 1.392(9) . ?
 C00C C00J 1.381(9) . ?
 C00D H00D 0.9500 . ?
 C00D C00E 1.394(8) . ?
 C00E H00E 0.9500 . ?
 C00E C00H 1.399(9) . ?
 N00F C00H 1.418(5) . ?
 N00F C00H 1.418(5) 12_654 ?
 N00F C00H 1.418(5) 6_665 ?
 C00G H00G 0.9500 . ?
 C00H C00K 1.397(9) . ?
 C00I H00I 0.9500 . ?
 C00I C00K 1.385(8) . ?
 C00J H00J 0.9500 . ?
 C00J C00L 1.368(8) . ?
 C00K H00K 0.9500 . ?
 C00L H00L 0.9500 . ?
 O00M H00M 0.8700 . ?
 O00M H00M 0.8701 2_665 ?

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
 C008 O002 H002 109.5 . . ?
 C00C N005 C00C 119.0(3) 8_656 . ?
 C00C N005 C00C 119.0(3) 11_566 . ?
 C00C N005 C00C 119.0(3) 8_656 11_566 ?
 H00A N006 H00C 109.5 . . ?
 H00A N006 H00F 109.5 . . ?
 H00A N006 H00H 109.5 . . ?
 H00C N006 H00F 109.4 . . ?
 H00C N006 H00H 109.5 . . ?
 H00F N006 H00H 109.5 . . ?
 O001 C007 C009 117.5(5) . . ?
 O003 C007 O001 123.9(5) . . ?
 O003 C007 C009 118.6(6) . . ?
 O002 C008 C00A 115.0(5) . . ?
 O004 C008 O002 123.5(5) . . ?
 O004 C008 C00A 121.5(6) . . ?
 C00D C009 C007 120.3(5) . . ?
 C00D C009 C00I 120.1(5) . . ?
 C00I C009 C007 119.6(5) . . ?
 C00B C00A C008 119.9(6) . . ?
 C00L C00A C008 120.9(6) . . ?
 C00L C00A C00B 119.2(5) . . ?
 C00A C00B H00B 119.7 . . ?
 C00A C00B C00G 120.5(6) . . ?
 C00G C00B H00B 119.7 . . ?
 C00G C00C N005 121.5(6) . . ?
 C00J C00C N005 119.7(7) . . ?
 C00J C00C C00G 118.9(5) . . ?
 C009 C00D H00D 119.5 . . ?
 C009 C00D C00E 120.9(6) . . ?
 C00E C00D H00D 119.5 . . ?
 C00D C00E H00E 120.5 . . ?
 C00D C00E C00H 119.1(6) . . ?
 C00H C00E H00E 120.5 . . ?
 C00H N00F C00H 119.49(17) 12_654 6_665 ?
 C00H N00F C00H 119.49(17) . 6_665 ?
 C00H N00F C00H 119.49(17) 12_654 . ?
 C00B C00G H00G 120.2 . . ?
 C00C C00G C00B 119.6(6) . . ?
 C00C C00G H00G 120.2 . . ?
 C00E C00H N00F 119.9(6) . . ?
 C00K C00H C00E 119.6(5) . . ?
 C00K C00H N00F 120.5(6) . . ?
 C009 C00I H00I 119.7 . . ?
 C009 C00I C00K 120.6(6) . . ?
 C00K C00I H00I 119.7 . . ?
 C00C C00J H00J 119.5 . . ?
 C00L C00J C00C 121.0(7) . . ?
 C00L C00J H00J 119.5 . . ?
 C00H C00K H00K 120.1 . . ?
 C00I C00K C00H 119.7(6) . . ?
 C00I C00K H00K 120.1 . . ?
 C00A C00L H00L 119.6 . . ?
 C00J C00L C00A 120.8(7) . . ?
 C00J C00L H00L 119.6 . . ?
 H00M O00M H00M 167.3 . 2_665 ?

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_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O001 C007 C009 C00D 12.5(9) . . . . ?
 O001 C007 C009 C00I -166.4(7) . . . . ?
 O002 C008 C00A C00B 9.1(10) . . . . ?
 O002 C008 C00A C00L -172.1(7) . . . . ?
 O003 C007 C009 C00D -167.4(7) . . . . ?
 O003 C007 C009 C00I 13.8(10) . . . . ?
 O004 C008 C00A C00B -169.6(7) . . . . ?
 O004 C008 C00A C00L 9.2(12) . . . . ?
 N005 C00C C00G C00B 179.4(9) . . . . ?
 N005 C00C C00J C00L -179.0(11) . . . . ?
 C007 C009 C00D C00E 178.9(7) . . . . ?
 C007 C009 C00I C00K 179.4(8) . . . . ?
 C008 C00A C00B C00G -179.3(7) . . . . ?
 C008 C00A C00L C00J 179.7(9) . . . . ?
 C009 C00D C00E C00H 1.9(11) . . . . ?
 C009 C00I C00K C00H 1.4(14) . . . . ?
 C00A C00B C00G C00C -0.6(13) . . . . ?
 C00B C00A C00L C00J -1.6(14) . . . . ?
 C00C N005 C00C C00G 133.7(10) 11_566 . . . ?
 C00C N005 C00C C00G -26(2) 8_656 . . . ?
 C00C N005 C00C C00J -46(2) 11_566 . . . ?
 C00C N005 C00C C00J 154.0(11) 8_656 . . . ?
 C00C C00J C00L C00A -0.1(18) . . . . ?
 C00D C009 C00I C00K 0.6(12) . . . . ?
 C00D C00E C00H N00F -179.1(8) . . . . ?
 C00D C00E C00H C00K 0.1(12) . . . . ?
 C00E C00H C00K C00I -1.7(14) . . . . ?
 N00F C00H C00K C00I 177.5(9) . . . . ?
 C00G C00C C00J C00L 1.4(17) . . . . ?
 C00H N00F C00H C00E -31.7(18) 12_654 . . . ?
 C00H N00F C00H C00E 134.2(9) 6_665 . . . ?
 C00H N00F C00H C00K -45.0(18) 6_665 . . . ?
 C00H N00F C00H C00K 149.1(10) 12_654 . . . ?
 C00I C009 C00D C00E -2.3(11) . . . . ?
 C00J C00C C00G C00B -1.0(14) . . . . ?
 C00L C00A C00B C00G 1.9(12) . . . . ?

_platon_squeeze_details            ?
_platon_squeeze_special_details
;
A solvent mask was calculated and 134 electrons were 
found in a volume of 1422Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.875[C3H7NO] per Unit Cell 
which account for 140 electrons 
per unit cell.
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
 1 0.000 0.000 0.000 711 67 '1.75 C3H7NO'
 2 0.500 0.500 0.500 711 67 '1.75 C3H7NO'

_platon_squeeze_void_probe_radius  1.20
_olex2_submission_special_instructions  'No special instructions were received'
