 
data_p3m1_sq
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C32 H26 Cu2 N2 O10' 
_chemical_formula_weight          725.63

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0060   0.0030
 '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'   0.0100   0.0050
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0180   0.0100
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cu'  'Cu'   0.1640   1.8640
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            164
_space_group_name_H-M_alt         'P -3 m 1'
_space_group_name_Hall            '-P 3 2"'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, z'
 
_cell_length_a                    23.515(3)
_cell_length_b                    23.515(3)
_cell_length_c                    11.052(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      5292.5(18)
_cell_formula_units_Z             3
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     573
_cell_measurement_theta_min       3.85
_cell_measurement_theta_max       25.83
 
_exptl_crystal_description        block
_exptl_crystal_colour             blue
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     0.683          
_exptl_crystal_F_000              1110
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.140
_exptl_crystal_size_mid           0.120
_exptl_crystal_size_min           0.080
_exptl_absorpt_coefficient_mu     1.139
_shelx_estimated_absorpt_T_min    0.857
_shelx_estimated_absorpt_T_max    0.914
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.88561
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       'Δφ scans'
_diffrn_reflns_number             41015
_diffrn_reflns_av_unetI/netI      0.0413
_diffrn_reflns_av_R_equivalents   0.0854
_diffrn_reflns_limit_h_min        -30
_diffrn_reflns_limit_h_max        30
_diffrn_reflns_limit_k_min        -30
_diffrn_reflns_limit_k_max        30
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          1.246
_diffrn_reflns_theta_max          35.098
_diffrn_reflns_theta_full         32.098
_diffrn_measured_fraction_theta_max   0.970
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.970
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.970
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              4222
_reflns_number_gt                 3530
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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.
;
 
_computing_data_collection        'marCCD 1994-2002'
_computing_cell_refinement        'XDSAPP 2.0 Sparta et al., 2016'
_computing_data_reduction         'XDSAPP 2.0 Sparta et al., 2016'
_computing_structure_solution     'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement   'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2500P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          4222
_refine_ls_number_parameters      112
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1120
_refine_ls_R_factor_gt            0.1039
_refine_ls_wR_factor_ref          0.3435
_refine_ls_wR_factor_gt           0.3214
_refine_ls_goodness_of_fit_ref    1.273
_refine_ls_restrained_S_all       1.273
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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 0.47360(2) 0.94721(2) 0.43213(5) 0.0580(3) Uani 1 2 d S T P . .
O1 O 0.51706(15) 0.91601(13) 0.5435(3) 0.0791(8) Uani 1 1 d . . . . .
O2 O 0.56077(16) 1.00495(13) 0.6607(3) 0.0814(8) Uani 1 1 d . . . . .
O3 O 0.43224(12) 0.8645(2) 0.3064(6) 0.1075(17) Uani 1 2 d S T P . .
H3O H 0.411517 0.823034 0.341814 0.129 Uiso 1 2 calc R U P . .
N1 N 0.6529(4) 0.8264(2) 0.9233(7) 0.150(4) Uani 1 2 d S T P . .
H1 H 0.677765 0.838883 0.986182 0.180 Uiso 1 2 calc R U P . .
C1 C 0.55025(19) 0.94857(16) 0.6335(3) 0.0718(9) Uani 1 1 d . . . . .
C2 C 0.5777(2) 0.91776(17) 0.7126(4) 0.0804(10) Uani 1 1 d . . . . .
C3 C 0.6156(3) 0.9516(2) 0.8147(6) 0.1133(19) Uani 1 1 d . . . . .
H3 H 0.622292 0.993248 0.831897 0.136 Uiso 1 1 calc R U . . .
C4 C 0.6420(4) 0.9257(3) 0.8873(6) 0.135(3) Uani 1 1 d . . . . .
H4 H 0.668230 0.949745 0.952204 0.162 Uiso 1 1 calc R U . . .
C5 C 0.6298(3) 0.8626(3) 0.8649(5) 0.1099(19) Uani 1 1 d . . . . .
C6 C 0.5948(3) 0.82836(19) 0.7609(5) 0.0911(14) Uani 1 1 d . . . . .
C7 C 0.5680(2) 0.85573(17) 0.6869(4) 0.0769(11) Uani 1 1 d . . . . .
H7 H 0.543478 0.832778 0.619673 0.092 Uiso 1 1 calc R U . . .
C8 C 0.4326(4) 0.8652(8) 0.2085(15) 0.271(11) Uani 1 2 d S T P . .
H8A H 0.479533 0.894314 0.199453 0.325 Uiso 0.5 1 calc R U P . .
H8B H 0.414781 0.894314 0.199453 0.325 Uiso 0.5 1 calc R U P . .
C9 C 0.4229(4) 0.8457(8) 0.1091(13) 0.293(12) Uani 1 2 d S T P . .
H9A H 0.441094 0.882189 0.054073 0.440 Uiso 1 2 calc R U P . .
H9B H 0.443078 0.819489 0.095816 0.440 Uiso 0.5 1 calc R U P . .
H9C H 0.376411 0.819489 0.095816 0.440 Uiso 0.5 1 calc 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
Cu1 O1 1.961(3) . ?
Cu1 O1 1.961(3) 11 ?
Cu1 O2 1.970(3) 5_676 ?
Cu1 O2 1.970(3) 7_676 ?
Cu1 O3 2.184(5) . ?
Cu1 Cu1 2.6219(10) 7_676 ?
O1 C1 1.260(5) . ?
O2 C1 1.257(4) . ?
O3 C8 1.083(16) . ?
N1 C5 1.376(6) . ?
N1 C5 1.376(6) 12_565 ?
C1 C2 1.475(5) . ?
C2 C7 1.389(5) . ?
C2 C3 1.411(6) . ?
C3 C4 1.333(8) . ?
C4 C5 1.387(7) . ?
C5 C6 1.409(6) . ?
C6 C7 1.372(6) . ?
C6 C6 1.457(8) 12_565 ?
C8 C9 1.167(17) . ?
 
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 90.15(19) . 11 ?
O1 Cu1 O2 89.67(14) . 5_676 ?
O1 Cu1 O2 168.42(12) 11 5_676 ?
O1 Cu1 O2 168.42(12) . 7_676 ?
O1 Cu1 O2 89.66(14) 11 7_676 ?
O2 Cu1 O2 88.2(2) 5_676 7_676 ?
O1 Cu1 O3 98.58(16) . . ?
O1 Cu1 O3 98.58(16) 11 . ?
O2 Cu1 O3 92.89(15) 5_676 . ?
O2 Cu1 O3 92.89(15) 7_676 . ?
O1 Cu1 Cu1 84.64(8) . 7_676 ?
O1 Cu1 Cu1 84.64(8) 11 7_676 ?
O2 Cu1 Cu1 83.82(8) 5_676 7_676 ?
O2 Cu1 Cu1 83.82(8) 7_676 7_676 ?
O3 Cu1 Cu1 175.40(17) . 7_676 ?
C1 O1 Cu1 123.3(2) . . ?
C1 O2 Cu1 123.9(3) . 7_676 ?
C8 O3 Cu1 128.7(9) . . ?
C5 N1 C5 109.1(5) . 12_565 ?
O2 C1 O1 124.4(4) . . ?
O2 C1 C2 118.2(3) . . ?
O1 C1 C2 117.4(3) . . ?
C7 C2 C3 118.8(4) . . ?
C7 C2 C1 120.9(3) . . ?
C3 C2 C1 120.3(4) . . ?
C4 C3 C2 122.0(4) . . ?
C3 C4 C5 119.1(4) . . ?
N1 C5 C4 130.1(5) . . ?
N1 C5 C6 109.2(4) . . ?
C4 C5 C6 120.4(4) . . ?
C7 C6 C5 119.5(4) . . ?
C7 C6 C6 134.3(2) . 12_565 ?
C5 C6 C6 106.2(3) . 12_565 ?
C6 C7 C2 119.9(4) . . ?
O3 C8 C9 159(2) . . ?
 
_refine_diff_density_max    1.287
_refine_diff_density_min   -1.551
_refine_diff_density_rms    0.148




