 
data_SCD22_118_Fddd_sq
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C44 H40 N14 Nd2 O10 [+anions + solvent]'
_chemical_formula_sum
 'C44 H40 N14 Nd2 O10 [+anions + solvent]' 
_chemical_formula_weight          	1213.38

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'
 'N'  'N'   0.0061   0.0033
 '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'
 'Nd'  'Nd'  -0.1943   3.0179
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            70
_space_group_name_H-M_alt         'F d d d'
_space_group_name_Hall            '-F 2uv 2vw'
 
_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'
 '-x+3/4, -y+3/4, z'
 '-x+3/4, y, -z+3/4'
 'x, -y+3/4, -z+3/4'
 'x, y+1/2, z+1/2'
 '-x+3/4, -y+5/4, z+1/2'
 '-x+3/4, y+1/2, -z+5/4'
 'x, -y+5/4, -z+5/4'
 'x+1/2, y, z+1/2'
 '-x+5/4, -y+3/4, z+1/2'
 '-x+5/4, y, -z+5/4'
 'x+1/2, -y+3/4, -z+5/4'
 'x+1/2, y+1/2, z'
 '-x+5/4, -y+5/4, z'
 '-x+5/4, y+1/2, -z+3/4'
 'x+1/2, -y+5/4, -z+3/4'
 '-x, -y, -z'
 'x-3/4, y-3/4, -z'
 'x-3/4, -y, z-3/4'
 '-x, y-3/4, z-3/4'
 '-x, -y+1/2, -z+1/2'
 'x-3/4, y-1/4, -z+1/2'
 'x-3/4, -y+1/2, z-1/4'
 '-x, y-1/4, z-1/4'
 '-x+1/2, -y, -z+1/2'
 'x-1/4, y-3/4, -z+1/2'
 'x-1/4, -y, z-1/4'
 '-x+1/2, y-3/4, z-1/4'
 '-x+1/2, -y+1/2, -z'
 'x-1/4, y-1/4, -z'
 'x-1/4, -y+1/2, z-3/4'
 '-x+1/2, y-1/4, z-3/4'
 
_cell_length_a                    13.9439(6)
_cell_length_b                    30.2750(15)
_cell_length_c                    31.0542(15)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      13109.6(11)
_cell_formula_units_Z             8
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used    5313
_cell_measurement_theta_min        2.54
_cell_measurement_theta_max       27.45

loop_
 _exptl_crystal_face_index_h
 _exptl_crystal_face_index_k
 _exptl_crystal_face_index_l
 _exptl_crystal_face_perp_dist
    1.00   -1.00    1.00    0.0120
    0.00    0.00    1.00    0.0120
    0.00    0.00   -1.00    0.0160
    0.00    2.00   -1.00    0.0100
    0.00   -2.00    1.00    0.0120
   -1.00   -1.00    0.00    0.0100
    1.00    1.00    0.00    0.0130
    1.00   -1.00   -1.00    0.0100
   -1.00    1.00    1.00    0.0160
  
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.230          
_exptl_crystal_F_000              4816
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.045
_exptl_crystal_size_mid           0.028
_exptl_crystal_size_min           0.025
_exptl_absorpt_coefficient_mu     1.619
_shelx_estimated_absorpt_T_min    0.931
_shelx_estimated_absorpt_T_max    0.961
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.4519
_exptl_absorpt_correction_T_max   0.4992
_exptl_absorpt_process_details    'SADABS, Bruker (2012)'
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             24530
_diffrn_reflns_av_unetI/netI      0.0421
_diffrn_reflns_av_R_equivalents   0.1036
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -37
_diffrn_reflns_limit_k_max        37
_diffrn_reflns_limit_l_min        -38
_diffrn_reflns_limit_l_max        38
_diffrn_reflns_theta_min          1.879
_diffrn_reflns_theta_max          26.000
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.990
_diffrn_measured_fraction_theta_full  0.990
_diffrn_reflns_Laue_measured_fraction_max    0.990
_diffrn_reflns_Laue_measured_fraction_full   0.990
_diffrn_reflns_point_group_measured_fraction_max   0.990
_diffrn_reflns_point_group_measured_fraction_full  0.990
_reflns_number_total              3205
_reflns_number_gt                 1868
_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      'Bruker SMART'
_computing_cell_refinement      'Bruker SMART'
_computing_data_reduction       'Bruker SAINT'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      heavy
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          3205
_refine_ls_number_parameters      161
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1436
_refine_ls_R_factor_gt            0.0994
_refine_ls_wR_factor_ref          0.3252
_refine_ls_wR_factor_gt           0.2813
_refine_ls_goodness_of_fit_ref    1.148
_refine_ls_restrained_S_all       1.148
_refine_ls_shift/su_max           0.000
_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
Nd1 Nd -0.1250 0.3750 0.69175(3) 0.0656(5) Uani 1 2 d S T P . .
O1 O -0.0474(4) 0.3712(2) 0.76223(16) 0.0400(14) Uani 1 1 d . . . . .
O2 O -0.1203(5) 0.4106(2) 0.62536(18) 0.0467(16) Uani 1 1 d . . . . .
O3 O -0.1250 0.3750 0.5632(2) 0.055(3) Uani 1 2 d S T P . .
N1 N -0.0804(5) 0.4557(2) 0.7099(2) 0.0394(17) Uani 1 1 d . . . . .
N2 N 0.0520(5) 0.3994(3) 0.6808(2) 0.0396(17) Uani 1 1 d . . . . .
N3 N 0.0115(5) 0.3140(2) 0.69037(18) 0.0342(17) Uani 1 1 d . . . . .
N4 N -0.1250 0.3750 0.6032(5) 0.063(4) Uani 1 2 d S T P . .
C1 C -0.1388(7) 0.4874(4) 0.7045(3) 0.051(3) Uani 1 1 d . . . . .
H1 H -0.1182 0.5165 0.7071 0.062 Uiso 1 1 calc R U . . .
C2 C 0.0200(7) 0.4667(4) 0.7184(4) 0.056(3) Uani 1 1 d . . . . .
H2A H 0.0413 0.4538 0.7454 0.067 Uiso 1 1 calc R U . . .
H2B H 0.0290 0.4984 0.7197 0.067 Uiso 1 1 calc R U . . .
C3 C 0.0739(8) 0.4470(4) 0.6807(4) 0.061(3) Uani 1 1 d . . . . .
H3A H 0.0530 0.4604 0.6539 0.073 Uiso 1 1 calc R U . . .
H3B H 0.1423 0.4518 0.6839 0.073 Uiso 1 1 calc R U . . .
C4 C 0.1233(7) 0.3718(4) 0.6797(3) 0.049(2) Uani 1 1 d . . . . .
H4 H 0.1862 0.3817 0.6768 0.059 Uiso 1 1 calc R U . . .
C5 C 0.1019(7) 0.3260(4) 0.6831(3) 0.045(2) Uani 1 1 d . . . . .
C6 C 0.1736(7) 0.2916(4) 0.6776(3) 0.059(3) Uani 1 1 d . . . . .
H6 H 0.2364 0.2996 0.6714 0.070 Uiso 1 1 calc R U . . .
C7 C 0.1524(9) 0.2504(5) 0.6813(3) 0.070(4) Uani 1 1 d . . . . .
H7 H 0.1995 0.2289 0.6776 0.084 Uiso 1 1 calc R U . . .
C8 C 0.0579(9) 0.2383(4) 0.6907(3) 0.062(3) Uani 1 1 d . . . . .
H8 H 0.0409 0.2088 0.6947 0.075 Uiso 1 1 calc R U . . .
C9 C -0.0108(8) 0.2724(3) 0.6939(3) 0.047(2) Uani 1 1 d . . . . .
C10 C -0.1250 0.3750 0.7813(3) 0.036(3) Uani 1 2 d S T P . .
C11 C -0.1250 0.3750 0.8305(3) 0.033(3) Uani 1 2 d S T P . .
C12 C -0.0385(6) 0.3756(3) 0.8524(3) 0.0375(19) Uani 1 1 d . . . . .
H12 H 0.0191 0.3767 0.8373 0.045 Uiso 1 1 calc R U . . .
 
 
_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
Nd1 O2 2.328(6) . y
Nd1 O2 2.328(6) 2_455 y
Nd1 O1 2.444(5) . y
Nd1 O1 2.444(5) 2_455 y
Nd1 N1 2.583(7) . y
Nd1 N1 2.583(7) 2_455 y
Nd1 N2 2.598(7) . y
Nd1 N2 2.598(7) 2_455 y
Nd1 N3 2.652(7) 2_455 y
Nd1 N3 2.652(7) . y
O1 C10 1.239(7) . ?
O2 N4 1.282(10) . ?
O3 N4 1.240(17) . ?
N1 C1 1.270(13) . ?
N1 C2 1.463(12) . ?
N2 C4 1.299(13) . ?
N2 C3 1.472(14) . ?
N3 C9 1.301(13) . ?
N3 C5 1.332(12) . ?
N4 O2 1.282(10) 2_455 ?
C1 C9 1.468(14) 2_455 ?
C1 H1 0.9300 . ?
C2 C3 1.515(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.423(16) . ?
C4 H4 0.9300 . ?
C5 C6 1.452(14) . ?
C6 C7 1.288(18) . ?
C6 H6 0.9300 . ?
C7 C8 1.400(18) . ?
C7 H7 0.9300 . ?
C8 C9 1.413(14) . ?
C8 H8 0.9300 . ?
C9 C1 1.468(14) 2_455 ?
C10 O1 1.239(7) 2_455 ?
C10 C11 1.528(14) . ?
C11 C12 1.385(10) 2_455 ?
C11 C12 1.385(10) . ?
C12 C12 1.406(16) 4_556 ?
C12 H12 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
O2 Nd1 O2 55.3(4) . 2_455 y
O2 Nd1 O1 143.4(2) . . y
O2 Nd1 O1 141.6(2) 2_455 . y
O2 Nd1 O1 141.6(2) . 2_455 y
O2 Nd1 O1 143.4(2) 2_455 2_455 y
O1 Nd1 O1 52.9(3) . 2_455 y
O2 Nd1 N1 75.4(2) . . y
O2 Nd1 N1 129.7(2) 2_455 . y
O1 Nd1 N1 75.1(2) . . y
O1 Nd1 N1 82.3(2) 2_455 . y
O2 Nd1 N1 129.7(2) . 2_455 y
O2 Nd1 N1 75.5(2) 2_455 2_455 y
O1 Nd1 N1 82.3(2) . 2_455 y
O1 Nd1 N1 75.1(2) 2_455 2_455 y
N1 Nd1 N1 154.7(3) . 2_455 y
O2 Nd1 N2 74.1(2) . . y
O2 Nd1 N2 92.4(2) 2_455 . y
O1 Nd1 N2 73.1(2) . . y
O1 Nd1 N2 121.6(2) 2_455 . y
N1 Nd1 N2 62.0(2) . . y
N1 Nd1 N2 121.7(2) 2_455 . y
O2 Nd1 N2 92.4(2) . 2_455 y
O2 Nd1 N2 74.1(2) 2_455 2_455 y
O1 Nd1 N2 121.6(2) . 2_455 y
O1 Nd1 N2 73.1(2) 2_455 2_455 y
N1 Nd1 N2 121.7(2) . 2_455 y
N1 Nd1 N2 62.0(2) 2_455 2_455 y
N2 Nd1 N2 165.0(3) . 2_455 y
O2 Nd1 N3 71.5(2) . 2_455 y
O2 Nd1 N3 106.7(2) 2_455 2_455 y
O1 Nd1 N3 111.43(19) . 2_455 y
O1 Nd1 N3 70.35(18) 2_455 2_455 y
N1 Nd1 N3 61.2(2) . 2_455 y
N1 Nd1 N3 119.3(2) 2_455 2_455 y
N2 Nd1 N3 118.8(2) . 2_455 y
N2 Nd1 N3 60.9(2) 2_455 2_455 y
O2 Nd1 N3 106.7(2) . . y
O2 Nd1 N3 71.5(2) 2_455 . y
O1 Nd1 N3 70.35(18) . . y
O1 Nd1 N3 111.43(19) 2_455 . y
N1 Nd1 N3 119.3(2) . . y
N1 Nd1 N3 61.2(2) 2_455 . y
N2 Nd1 N3 60.9(2) . . y
N2 Nd1 N3 118.8(2) 2_455 . y
N3 Nd1 N3 178.1(2) 2_455 . y
C10 O1 Nd1 92.0(5) . . ?
N4 O2 Nd1 94.9(7) . . ?
C1 N1 C2 117.8(9) . . ?
C1 N1 Nd1 122.0(6) . . ?
C2 N1 Nd1 119.0(6) . . ?
C4 N2 C3 118.0(8) . . ?
C4 N2 Nd1 123.3(6) . . ?
C3 N2 Nd1 118.4(6) . . ?
C9 N3 C5 120.3(8) . . ?
C9 N3 Nd1 120.1(6) . . ?
C5 N3 Nd1 119.4(6) . . ?
O3 N4 O2 122.5(6) . 2_455 ?
O3 N4 O2 122.5(6) . . ?
O2 N4 O2 114.9(12) 2_455 . ?
N1 C1 C9 119.3(9) . 2_455 ?
N1 C1 H1 120.3 . . ?
C9 C1 H1 120.3 2_455 . ?
N1 C2 C3 104.2(8) . . ?
N1 C2 H2A 110.9 . . ?
C3 C2 H2A 110.9 . . ?
N1 C2 H2B 110.9 . . ?
C3 C2 H2B 110.9 . . ?
H2A C2 H2B 108.9 . . ?
N2 C3 C2 106.3(8) . . ?
N2 C3 H3A 110.5 . . ?
C2 C3 H3A 110.5 . . ?
N2 C3 H3B 110.5 . . ?
C2 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N2 C4 C5 117.6(8) . . ?
N2 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
N3 C5 C4 118.5(8) . . ?
N3 C5 C6 118.4(10) . . ?
C4 C5 C6 123.0(10) . . ?
C7 C6 C5 121.8(11) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C8 119.2(11) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C9 C8 C7 117.4(11) . . ?
C9 C8 H8 121.3 . . ?
C7 C8 H8 121.3 . . ?
N3 C9 C8 122.7(10) . . ?
N3 C9 C1 116.2(8) . 2_455 ?
C8 C9 C1 121.0(10) . 2_455 ?
O1 C10 O1 123.0(9) 2_455 . ?
O1 C10 C11 118.5(5) 2_455 . ?
O1 C10 C11 118.5(5) . . ?
C12 C11 C12 121.2(10) 2_455 . ?
C12 C11 C10 119.4(5) 2_455 . ?
C12 C11 C10 119.4(5) . . ?
C12 C12 C11 119.4(5) 4_556 . ?
C12 C12 H12 120.3 4_556 . ?
C11 C12 H12 120.3 . . ?
 
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_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
Nd1 O2 N4 O3 180.000(2) . . . . ?
Nd1 O2 N4 O2 0.001(2) . . . 2_455 ?
C2 N1 C1 C9 177.2(8) . . . 2_455 ?
Nd1 N1 C1 C9 9.7(12) . . . 2_455 ?
C1 N1 C2 C3 -117.7(10) . . . . ?
Nd1 N1 C2 C3 50.3(10) . . . . ?
C4 N2 C3 C2 -128.0(9) . . . . ?
Nd1 N2 C3 C2 45.4(10) . . . . ?
N1 C2 C3 N2 -58.3(11) . . . . ?
C3 N2 C4 C5 175.4(8) . . . . ?
Nd1 N2 C4 C5 2.4(12) . . . . ?
C9 N3 C5 C4 -179.6(7) . . . . ?
Nd1 N3 C5 C4 4.9(10) . . . . ?
C9 N3 C5 C6 2.4(12) . . . . ?
Nd1 N3 C5 C6 -173.1(6) . . . . ?
N2 C4 C5 N3 -4.9(13) . . . . ?
N2 C4 C5 C6 173.1(9) . . . . ?
N3 C5 C6 C7 -2.7(14) . . . . ?
C4 C5 C6 C7 179.4(10) . . . . ?
C5 C6 C7 C8 0.0(16) . . . . ?
C6 C7 C8 C9 2.7(15) . . . . ?
C5 N3 C9 C8 0.4(12) . . . . ?
Nd1 N3 C9 C8 175.9(7) . . . . ?
C5 N3 C9 C1 176.5(8) . . . 2_455 ?
Nd1 N3 C9 C1 -8.1(9) . . . 2_455 ?
C7 C8 C9 N3 -3.0(14) . . . . ?
C7 C8 C9 C1 -178.9(9) . . . 2_455 ?
Nd1 O1 C10 O1 -0.002(2) . . . 2_455 ?
Nd1 O1 C10 C11 180.000(2) . . . . ?
O1 C10 C11 C12 6.9(5) 2_455 . . 2_455 ?
O1 C10 C11 C12 -173.1(5) . . . 2_455 ?
O1 C10 C11 C12 -173.1(5) 2_455 . . . ?
O1 C10 C11 C12 6.9(5) . . . . ?
C12 C11 C12 C12 1.6(8) 2_455 . . 4_556 ?
C10 C11 C12 C12 -178.4(8) . . . 4_556 ?

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 -0.004 -0.003 -0.003      5082      1198 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

_refine_diff_density_max    1.515
_refine_diff_density_min   -0.839
_refine_diff_density_rms    0.262




