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_4516558
_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         'C122 H85 Dy3 N8 O41, 4(H2 O)'
_chemical_formula_sum            'C122 H93 Dy3 N8 O45'
_chemical_formula_weight         2878.54
_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             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                   14.9189(5)
_cell_length_b                   14.9189(5)
_cell_length_c                   55.485(4)
_cell_measurement_reflns_used    8783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.005
_cell_measurement_theta_min      2.425
_cell_volume                     12349.5(11)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.631 (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 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  0.0929
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            88923
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         1.413
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.888
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       pyramid
_exptl_crystal_F_000             5756
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Flack x determined using 3893 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         10917
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+32.5376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10058
_reflns_number_total             10917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5b01387_si_002.cif
_cod_data_source_block           7
_cod_original_cell_volume        12349.5(12)
_cod_database_code               4516558
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C13C, C13Z}
3. Restrained distances
 C14C-O3C = C14Z-O3Z
 1.45 with sigma of 0.01
 O6-C1S
 1.45 with sigma of 0.01
 C1S-C2S
 1.54 with sigma of 0.02
 C1BA-C1BB
 0.25 with sigma of 0.02
 O1A-O3Z_$1
 2.7 with sigma of 0.02
 C13C-C14C \\sim C13Z-C14Z
 with sigma of 0.01
 O1BB-C1BB \\sim O1BA-C1BA
 with sigma of 0.015
 N1B-C1BA \\sim N1B-C1BB
 with sigma of 0.01
 C2B-C1BA \\sim C2B-C1BB
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N1A) \\sim Ueq, Uanis(C5C) \\sim Ueq, Uanis(C9C) \\sim Ueq, Uanis(C4D)
\\sim Ueq, Uanis(C2D) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C4C) \\sim Ueq,
Uanis(O5A) \\sim Ueq, Uanis(O3D) \\sim Ueq, Uanis(C3D) \\sim Ueq, Uanis(C10C)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uiso(C13C) = Uiso(C13Z)
Uiso(C14C) = Uiso(O3C) = Uiso(C14Z) = Uiso(O3Z)
Uanis(O1BA) = Uanis(O1BB)
Uiso(C1BA) = Uiso(C1BB)
5. Others
 Fixed Sof: C1BA(0.5) C1BB(0.5) O1BA(0.5) O1BB(0.5) 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) O6(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) H2SC(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), C1S(H1SA,H1SB)
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)
6.d Idealised Me refined with riding coordinates:
 C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              30140
_shelx_hkl_checksum              68780
_shelx_fab_checksum              33756
_olex2_submission_special_instructions 'No special instructions were received'