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_4516559
_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 Ce2.27 N8 O41 Tb0.73, 4(H2 O)'
_chemical_formula_sum            'C120 H89 Ce2.27 N8 O45 Tb0.73'
_chemical_formula_weight         2797.16
_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     heavy
_audit_creation_date             2015-03-17
_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                   14.8679(16)
_cell_length_b                   14.8679(16)
_cell_length_c                   55.353(6)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.785
_cell_measurement_theta_min      2.293
_cell_volume                     12236(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            34607
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        23.950
_diffrn_reflns_theta_max         23.947
_diffrn_reflns_theta_min         2.230
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.4831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1334 before and 0.0790 after correction.
The Ratio of minimum to maximum transmission is 0.6485.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       prism
_exptl_crystal_F_000             5617
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details
;
 Flack x determined using 2582 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(11)
_refine_ls_extinction_coef       0.00074(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         9451
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+23.2538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                7472
_reflns_number_total             9451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b01387_si_002.cif
_cod_data_source_block           8
_cod_original_cell_volume        12236(3)
_cod_database_code               4516559
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.824
_shelx_estimated_absorpt_t_min   0.739
_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, Ce1}
{Tb2, 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
Uanis(C1A) \\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uiso(C13C) = Uiso(C13Z)
Uiso(C14C) = Uiso(O3C) = Uiso(C14Z) = Uiso(O3Z)
Uanis(Tb1) = Uanis(Ce1)
Uanis(Tb2) = Uanis(Ce2)
Uiso(O6A) = Uiso(O6B)
5. Others
 Sof(O6B)=0.5*(1-FVAR(2))
 Sof(O6A)=0.5*FVAR(2)
 Sof(Ce1)=1-FVAR(2)
 Sof(Tb1)=FVAR(2)
 Sof(Ce2)=0.5*(1-FVAR(4))
 Sof(Tb2)=0.5*FVAR(4)
 Fixed Sof: C13C(0.6) H13C(0.6) C14C(0.6) H14E(0.6) H14F(0.6) O3C(0.6)
 C13Z(0.4) H13Z(0.4) C14Z(0.4) H14G(0.4) H14H(0.4) O3Z(0.4)
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              63697
_shelx_hkl_checksum              76267
_shelx_fab_checksum              95370
_olex2_submission_special_instructions 'No special instructions were received'