Synthesis, structure, and photoluminescent behaviour of molecular lanthanide‒2-thiophenecarboxylate‒2,2′:6′,2′′-terpyridine materials
Batrice, Rami J.; Ridenour, J. August; Ayscue III, R. Lee; Bertke, Jeffery A.; Knope, Karah E.; CrystEngComm  (2017) –; doi:10.1039/C7CE01192J

data_7228979
_publ_section_title
;
 Synthesis, structure, and photoluminescent behaviour of molecular
 lanthanide--2-thiophenecarboxylate--2,2&#x2032;:6&#x2032;,2&#x2032;&#x2032;-terpyridine
 materials
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01192J
_journal_year                    2017
_chemical_formula_moiety         'C60 H44 Gd2 N6 O14 S6, 0.37(H2 O)'
_chemical_formula_sum            'C60 H44.74 Gd2 N6 O14.37 S6'
_chemical_formula_weight         1586.54
_chemical_name_systematic        'Gd Dimer'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-04-06
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.852(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9100(5)
_cell_length_b                   25.3890(10)
_cell_length_c                   9.7186(4)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.26
_cell_volume                     2911.2(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26054
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.099
_diffrn_reflns_theta_min         2.262
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_T_max  0.9166
_exptl_absorpt_correction_T_min  0.8219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0881 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.8967.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1571
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     1045
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0155P)^2^+1.6699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5388
_reflns_number_total             6426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01192j2.cif
_cod_data_source_block           final_a_CCDC13
_cod_database_code               7228979
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.807
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B
 0.86 with sigma of 0.02
 O8-H8B = O8-H8A
 0.86 with sigma of 0.02
 H7A-H7B
 1.35 with sigma of 0.02
 H8B-H8A
 1.35 with sigma of 0.02
 S1-C17 \\sim S1A-C17 \\sim S2A-C22 \\sim S2-C22 \\sim S3-C27 \\sim S3A-C27
 with sigma of 0.01
 S1-C20 \\sim S1A-C20A \\sim S2A-C25A \\sim S2-C25 \\sim S3-C30 \\sim S3A-C30A
 with sigma of 0.01
 C30A-C29A \\sim C30-C29 \\sim C25-C24 \\sim C25A-C24A \\sim C20A-C19A \\sim
C20-C19
 with sigma of 0.01
 C18-C17 \\sim C18A-C17 \\sim C23-C22 \\sim C23A-C22 \\sim C28-C27 \\sim
C28A-C27
 with sigma of 0.01
 C24A-C23A \\sim C24-C23 \\sim C19-C18 \\sim C19A-C18A \\sim S3A-C30A \\sim
C29A-C28A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim S1A \\sim C18A \\sim C19A
\\sim C20A \\sim S1 \\sim C17 \\sim C18 \\sim C17 \\sim S1A \\sim C17 \\sim
C18A \\sim C17 \\sim S1 \\sim C20 \\sim C19 \\sim C18 \\sim S1A \\sim C20A
\\sim C19A \\sim C18A \\sim C20 \\sim C19 \\sim C20A \\sim C19A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim S2A \\sim C23A \\sim C24A
\\sim C25A \\sim S2 \\sim C22 \\sim C23 \\sim C22 \\sim S2A \\sim C22 \\sim
C23A \\sim C22 \\sim S2 \\sim C25 \\sim C24 \\sim C23 \\sim S2A \\sim C25A
\\sim C24A \\sim C23A \\sim C25 \\sim C24 \\sim C25A \\sim C24A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim S3A \\sim C28A \\sim C29A
\\sim C30A \\sim S3 \\sim C27 \\sim C28 \\sim C27 \\sim S3A \\sim C27 \\sim
C28A \\sim C27 \\sim S3 \\sim C30 \\sim C29 \\sim C28 \\sim S3A \\sim C30A
\\sim C29A \\sim C28A \\sim C30 \\sim C29 \\sim C30A \\sim C29A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C28(H28), C29(H29), C30(H30), C18A(H18A), C19A(H19A), C20A(H20A), C23A(H23A),
 C24A(H24A), C25A(H25A), C28A(H28A), C29A(H29A), C30A(H30A)
;
_olex2_submission_original_sample_id RJB390
_olex2_submission_special_instructions 'No special instructions were received'