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_7228973
_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         'C60 H44 Ho2 N6 O14 S6, 0.32(H2 O)'
_chemical_formula_sum            'C60 H44.63 Ho2 N6 O14.32 S6'
_chemical_formula_weight         1600.90
_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                 97.574(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.8674(6)
_cell_length_b                   25.2352(12)
_cell_length_c                   9.7280(5)
_cell_measurement_reflns_used    9129
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.58
_cell_measurement_theta_min      2.37
_cell_volume                     2887.9(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 0.994
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            32543
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.261
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.012
_exptl_absorpt_correction_T_max  0.6838
_exptl_absorpt_correction_T_min  0.3920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1070 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.5733.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_description       block
_exptl_crystal_F_000             1582
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.203
_refine_diff_density_max         0.621
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     1008
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0137P)^2^+3.4795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5728
_reflns_number_total             6348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01192j2.cif
_cod_data_source_block           final_a_CCDC7
_cod_database_code               7228973
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.580
_shelx_estimated_absorpt_t_min   0.337
_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
 H7A-H7B
 1.35 with sigma of 0.02
 H8A-H8B
 1.35 with sigma of 0.02
 S3A-C27 \\sim S3-C27 \\sim S1A-C17 \\sim S1-C17 \\sim S2-C22 \\sim S2A-C22
 with sigma of 0.01
 S3A-C30A \\sim S3-C30 \\sim S1-C20 \\sim S1A-C20A \\sim S2A-C25A \\sim S2-C25
 with sigma of 0.01
 C30A-C29A \\sim C30-C29 \\sim C20A-C19A \\sim C20-C19 \\sim C25A-C24A \\sim
C25-C24
 with sigma of 0.01
 C23-C22 \\sim C23A-C22 \\sim C18A-C17 \\sim C18-C17 \\sim C28A-C27 \\sim
C28-C27
 with sigma of 0.01
 C24-C23 \\sim C24A-C23A \\sim C19A-C18A \\sim C19-C18 \\sim C29A-C28A \\sim
C29-C28
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S2 \\sim S2 \\sim S2 \\sim C22 \\sim C22 \\sim C22 \\sim C22 \\sim C22 \\sim
C23 \\sim C23 \\sim C23 \\sim C24 \\sim C24 \\sim C24 \\sim C25 \\sim C25 \\sim
C25 \\sim S2A \\sim S2A \\sim S2A \\sim C23A \\sim C23A \\sim C23A \\sim C24A
\\sim C24A \\sim C24A \\sim C25A \\sim C25A \\sim C25A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
S1 \\sim S1 \\sim S1 \\sim C17 \\sim C17 \\sim C17 \\sim C17 \\sim C17 \\sim
C18 \\sim C18 \\sim C18 \\sim C19 \\sim C19 \\sim C19 \\sim C20 \\sim C20 \\sim
C20 \\sim S1A \\sim S1A \\sim S1A \\sim C18A \\sim C18A \\sim C18A \\sim C19A
\\sim C19A \\sim C19A \\sim C20A \\sim C20A \\sim C20A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3 \\sim S3 \\sim C27 \\sim C27 \\sim C27 \\sim C27 \\sim C27 \\sim
C28 \\sim C28 \\sim C28 \\sim C29 \\sim C29 \\sim C29 \\sim C30 \\sim C30 \\sim
C30 \\sim S3A \\sim S3A \\sim S3A \\sim C28A \\sim C28A \\sim C28A \\sim C29A
\\sim C29A \\sim C29A \\sim C30A \\sim C30A \\sim C30A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
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'