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_7228976
_publ_section_title
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 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         'C60 H44 Ce2 N6 O14 S6, 0.69(H2 O)'
_chemical_formula_sum            'C60 H45.39 Ce2 N6 O14.69 S6'
_chemical_formula_weight         1558.14
_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                 98.2700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0450(6)
_cell_length_b                   25.8165(12)
_cell_length_c                   9.6836(4)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.27
_cell_volume                     2979.9(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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            34525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.146
_diffrn_reflns_theta_min         2.326
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.792
_exptl_absorpt_correction_T_max  0.8512
_exptl_absorpt_correction_T_min  0.5690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.6685.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.519
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6588
_refine_ls_number_restraints     1002
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0153P)^2^+2.5824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5802
_reflns_number_total             6588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01192j2.cif
_cod_data_source_block           final_a_CCDC10
_cod_database_code               7228976
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.456
_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-H8A = O8-H8B
 0.86 with sigma of 0.02
 H8A-H8B
 1.35 with sigma of 0.02
 H7B-H7A
 1.35 with sigma of 0.02
 S3A-C27 \\sim S3-C27 \\sim S2-C22 \\sim S2A-C22 \\sim S1A-C17 \\sim S1-C17
 with sigma of 0.01
 S3A-C30A \\sim S3-C30 \\sim S2-C25 \\sim S2A-C25A \\sim S1-C20 \\sim S1A-C20A
 with sigma of 0.01
 C20-C19 \\sim C20A-C19A \\sim C25-C24 \\sim C25A-C24A \\sim C30-C29 \\sim
C30A-C29A
 with sigma of 0.01
 C28-C27 \\sim C28A-C27 \\sim C23A-C22 \\sim C23-C22 \\sim C18A-C17 \\sim
C18-C17
 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 S1A \\sim C17 \\sim C18 \\sim C18A \\sim C19 \\sim C19A \\sim C20
\\sim C20A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim S2A \\sim C22 \\sim C23 \\sim C23A \\sim C24 \\sim C24A \\sim C25
\\sim C25A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3A \\sim C27 \\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
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), 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'