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_4516561
_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 H81 Ce1.41 Gd0.27 N8 O41 Tb1.32, 4(H2 O)'
_chemical_formula_sum            'C120 H89 Ce1.41 Gd0.27 N8 O45 Tb1.32'
_chemical_formula_weight         2812.79
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9837(7)
_cell_length_b                   14.9837(7)
_cell_length_c                   55.753(5)
_cell_measurement_reflns_used    9426
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.878
_cell_measurement_theta_min      2.652
_cell_volume                     12517.2(14)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area 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  0.0796
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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            134466
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.070
_diffrn_reflns_theta_min         1.407
_exptl_absorpt_coefficient_mu    1.472
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             5643
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 3806 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         11101
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0521P)^2^+4.4027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9911
_reflns_number_total             11101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b01387_si_002.cif
_cod_data_source_block           10
_cod_original_cell_volume        12517.3(17)
_cod_database_code               4516561
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.719
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C13C, C13Z}
{Tb1, Gd1, Ce1}
{Tb2, Gd2, Ce2}
3. Restrained distances
 C14C-O3C = C14Z-O3Z
 1.45 with sigma of 0.01
 O1A-O3Z_$1
 -2.75 with sigma of 0.015
 Tb2-O6B
 2.36 with sigma of 0.01
 C13C-C14C \\sim C13Z-C14Z
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uiso(C13C) = Uiso(C13Z)
Uiso(C14C) = Uiso(O3C) = Uiso(C14Z) = Uiso(O3Z)
Uanis(Tb1) = Uanis(Gd1) = Uanis(Ce1)
Uanis(Tb2) = Uanis(Gd2) = Uanis(Ce2)
Uiso(O6A) = Uiso(O6B)
5. Others
 Sof(O6B)=0.5*(1-FVAR(2))
 Sof(O6A)=0.5*FVAR(2)
 Fixed Sof: Tb1(0.44) Gd1(0.09) Ce1(0.47) Tb2(0.22) Gd2(0.045) Ce2(0.235)
 C13C(0.5) H13C(0.5) C14C(0.5) H14E(0.5) H14F(0.5) O3C(0.5) C13Z(0.5) H13Z(0.5)
 C14Z(0.5) H14G(0.5) H14H(0.5) O3Z(0.5)
6.a Ternary CH refined with riding coordinates:
 C13A(H13A), C13B(H13B), C13C(H13C), C13Z(H13Z), C13D(H13D)
6.b Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B), C14B(H14C,H14D), C14C(H14E,H14F), C14Z(H14G,H14H), C14D(H14I,
 H14J)
6.c 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)
;
_shelx_res_checksum              78086
_shelx_hkl_checksum              55648
_shelx_fab_checksum              56290
_olex2_submission_special_instructions 'No special instructions were received'