Homochiral, Helical Coordination Complexes of Lanthanides(III) and Mixed-Metal Lanthanides(III): Impact of the 1,8-Naphthalimide Supramolecular Tecton on Structure, Magnetic Properties, and Luminescence
Reger, Daniel L.; Leitner, Andrew; Smith, Mark D.; Crystal Growth & Design 15 (2015) 5637–; doi:10.1021/acs.cgd.5b01387

data_4516553
_publ_section_title
;
 Homochiral, Helical Coordination Complexes of Lanthanides(III) and
 Mixed-Metal Lanthanides(III): Impact of the 1,8-Naphthalimide
 Supramolecular Tecton on Structure, Magnetic Properties, and Luminescence
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5637
_journal_paper_doi               10.1021/acs.cgd.5b01387
_journal_volume                  15
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C120 H83 Ce3 N8 O42, 4(H2 O)'
_chemical_formula_sum            'C120 H91 Ce3 N8 O46'
_chemical_formula_weight         2801.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0749(10)
_cell_length_b                   15.0749(10)
_cell_length_c                   55.646(7)
_cell_measurement_reflns_used    7339
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      2.41
_cell_volume                     12646(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD are detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            159891
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.013
_diffrn_reflns_theta_max         25.013
_diffrn_reflns_theta_min         1.399
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       plate
_exptl_crystal_F_000             5636
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 4178 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         11142
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0368
_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/[\s^2^(Fo^2^)+(0.0469P)^2^+4.0675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10591
_reflns_number_total             11142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b01387_si_002.cif
_cod_data_source_block           2
_cod_database_code               4516553
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O1A-O3CB_$1
 -2.7 with sigma of 0.015
 O7-O3E
 -2.7 with sigma of 0.02
 C14C-O3CA = C14C-O3CB = C14Z-O3CC
 1.45 with sigma of 0.02
 C13C-C15C \\sim C13Z-C15C
 with sigma of 0.01
 N1C-C13C \\sim N1C-C13Z
 with sigma of 0.01
 N1C-C14C \\sim N1C-C14Z
 with sigma of 0.01
 C13C-C14C \\sim C13Z-C14Z
 with sigma of 0.0075
3. Uiso/Uaniso restraints and constraints
Uiso(O3CA) = Uiso(O3CB) = Uiso(O3CC)
Uiso(C13D) = Uiso(C13E)
Uiso(C15D) = Uiso(C15E)
Uanis(O4D) = Uanis(O4E)
Uiso(N1D) = Uiso(N1E)
Uiso(C10D) = Uiso(C11D) = Uiso(C11E)
Uiso(C8D) = Uiso(C8E)
Uiso(C9D) = Uiso(C9E)
Uiso(C2D) = Uiso(C2E)
Uiso(C5D) = Uiso(C5E)
Uiso(C4D) = Uiso(C4E)
Uanis(O3D) = Uanis(O3E)
Uanis(O2D) = Uanis(O2E)
Uiso(C3D) = Uiso(C3E)
Uiso(C14C) = Uiso(C14Z)
Uiso(C13C) = Uiso(C13Z)
Uiso(O5D) = Uiso(O5E)
4. Same fragment restrains
{C1D, C2D, C3D, C4D, C5D, C6D, C7D, C8D, C9D, C10D, C11D, C12D, C13D, C14D,
C15D, N1D, O1D, O2D, O3D, O4D, O5D} sigma for 1-2: 0.015, 1-3: 0.04
as
{C1E, C2E, C3E, C4E, C5E, C6E, C7E, C8E, C9E, C10E, C11E, C12E, C13E, C14E,
C15E, N1E, O1E, O2E, O3E, O4E, O5E}
5. Others
 1*[Sof(H14E)+Sof(H14F)+Sof(O3CA)]+1*[Sof(H14G)+Sof(H14H)+Sof(O3CB)]+1*
 [Sof(C13C)+Sof(H13C)+Sof(C14C)+Sof(C13Z)+Sof(H13Z)+Sof(C14Z)+Sof(H14I)+
 Sof(H14J)+Sof(O3CC)]=1 with esd of 0.0001
 Sof(C1E)=Sof(C2E)=Sof(C3E)=Sof(C4E)=Sof(C5E)=Sof(C6E)=Sof(H6E)=Sof(C7E)=
 Sof(H7E)=Sof(C8E)=Sof(H8E)=Sof(C9E)=Sof(C10E)=Sof(H10E)=Sof(C11E)=Sof(H11E)=
 Sof(C12E)=Sof(H12E)=Sof(C13E)=Sof(H13E)=Sof(C14E)=Sof(H14M)=Sof(H14N)=
 Sof(C15E)=Sof(N1E)=Sof(O1E)=Sof(O2E)=Sof(O3E)=Sof(O4E)=Sof(O5E)=1-FVAR(1)
 Sof(C1D)=Sof(C2D)=Sof(C3D)=Sof(C4D)=Sof(C5D)=Sof(C6D)=Sof(H6D)=Sof(C7D)=
 Sof(H7D)=Sof(C8D)=Sof(H8D)=Sof(C9D)=Sof(C10D)=Sof(H10D)=Sof(C11D)=Sof(H11D)=
 Sof(C12D)=Sof(H12D)=Sof(C13D)=Sof(H13D)=Sof(C14D)=Sof(H14K)=Sof(H14L)=
 Sof(C15D)=Sof(N1D)=Sof(O1D)=Sof(O2D)=Sof(O3D)=Sof(O4D)=Sof(O5D)=FVAR(1)
 Sof(H14E)=Sof(H14F)=Sof(O3CA)=FVAR(2)
 Sof(H14G)=Sof(H14H)=Sof(O3CB)=FVAR(3)
 Sof(C13C)=Sof(H13C)=Sof(C14C)=1-FVAR(4)
 Sof(C13Z)=Sof(H13Z)=Sof(C14Z)=Sof(H14I)=Sof(H14J)=Sof(O3CC)=FVAR(4)
6.a Riding coordinates:
 C14C(H14E,H14F,H14G,H14H)
6.b Ternary CH refined with riding coordinates:
 C13A(H13A), C13B(H13B), C13C(H13C), C13Z(H13Z), C13D(H13D), C13E(H13E)
6.c Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B), C14B(H14C,H14D), C14Z(H14I,H14J), C14D(H14K,H14L), C14E(H14M,
 H14N)
6.d Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A), C12A(H12A), C6B(H6B),
 C7B(H7B), C8B(H8B), C10B(H10B), C11B(H11B), C12B(H12B), C6C(H6C), C7C(H7C),
 C8C(H8C), C10C(H10C), C11C(H11C), C12C(H12C), C6D(H6D), C7D(H7D), C8D(H8D),
 C10D(H10D), C11D(H11D), C12D(H12D), C6E(H6E), C7E(H7E), C8E(H8E), C10E(H10E),
 C11E(H11E), C12E(H12E)
;
_shelx_res_checksum              94681
_shelx_hkl_checksum              74100
_shelx_fab_checksum              69890
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'