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_7228971
_publ_section_title
;
 Synthesis, structure, and photoluminescent behaviour of molecular
 lanthanide--2-thiophenecarboxylate--2,2&#x2032;:6&#x2032;,2&#x2032;&#x2032;-terpyridine
 materials
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01192J
_journal_year                    2017
_chemical_formula_moiety         'C30 H22 Lu N3 O7 S3'
_chemical_formula_sum            'C30 H22 Lu N3 O7 S3'
_chemical_formula_weight         807.65
_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
_atom_sites_solution_primary     dual
_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                 98.219(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4315(5)
_cell_length_b                   20.2753(12)
_cell_length_c                   17.5412(11)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.33
_cell_volume                     2967.9(3)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49796
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.326
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.591
_exptl_absorpt_correction_T_max  0.8282
_exptl_absorpt_correction_T_min  0.4421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1225 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.5338.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.431
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6067
_refine_ls_number_restraints     986
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+4.0809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5596
_reflns_number_total             6067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01192j2.cif
_cod_data_source_block           final_a_CCDC5
_cod_database_code               7228971
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.387
_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
 S1A-C17 \\sim S1-C17 \\sim S2-C22 \\sim S2A-C22 \\sim S3-C27 \\sim S3A-C27
 with sigma of 0.01
 S1A-C20A \\sim S1-C20 \\sim S2-C25 \\sim S2A-C25A \\sim S3-C30 \\sim S3A-C30A
 with sigma of 0.01
 C30-C29 \\sim C30A-C29A \\sim C25A-C24A \\sim C25-C24 \\sim C20-C19 \\sim
C20A-C19A
 with sigma of 0.01
 C28-C27 \\sim C28A-C27 \\sim C18-C17 \\sim C18A-C17 \\sim C23A-C22 \\sim
C23-C22
 with sigma of 0.01
 C29A-C28A \\sim C29-C28 \\sim C24A-C23A \\sim C24-C23 \\sim C19A-C18A \\sim
C19-C18
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim S1 \\sim S1 \\sim S1A \\sim S1A \\sim S1A \\sim C17 \\sim C17 \\sim
C17 \\sim C17 \\sim C17 \\sim C18 \\sim C18 \\sim C18 \\sim C18A \\sim C18A
\\sim C18A \\sim C19 \\sim C19 \\sim C19 \\sim C19A \\sim C19A \\sim C19A \\sim
C20 \\sim C20 \\sim C20 \\sim C20A \\sim C20A \\sim C20A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim S2 \\sim S2 \\sim S2A \\sim S2A \\sim S2A \\sim C22 \\sim C22 \\sim
C22 \\sim C22 \\sim C22 \\sim C23 \\sim C23 \\sim C23 \\sim C23A \\sim C23A
\\sim C23A \\sim C24 \\sim C24 \\sim C24 \\sim C24A \\sim C24A \\sim C24A \\sim
C25 \\sim C25 \\sim C25 \\sim C25A \\sim C25A \\sim C25A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3A \\sim C28 \\sim C28A \\sim C29 \\sim C29A \\sim C30 \\sim C30A:
within 2A 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
Uanis(C18) \\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)
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), C18A(H18A), C19(H19), C19A(H19A), C20(H20),
 C20A(H20A), C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A),
 C28(H28), C28A(H28A), C29(H29), C29A(H29A), C30(H30), C30A(H30A)
;
_olex2_submission_special_instructions 'No special instructions were received'