Synthesis and characterization of thallium-salen derivatives for use as underground fluid flow tracers.
Boyle, Timothy J.; Perales, Diana; Rimsza, Jessica M.; Alam, Todd M.; Boye, Daniel M.; Sears, Jeremiah M.; Greathouse, Jeffery A.; Kemp, Richard A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4162–4174; doi:10.1039/c7dt04121g

data_7045677
_publ_section_title
;
 Synthesis and characterization of thallium-salen derivatives for use as
 underground fluid flow tracers.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4162
_journal_page_last               4174
_journal_paper_doi               10.1039/c7dt04121g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C32 H46 N2 O2 Tl2'
_chemical_formula_sum            'C32 H46 N2 O2 Tl2'
_chemical_formula_weight         899.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-20 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1980(2)
_cell_length_b                   19.1223(6)
_cell_length_c                   27.6952(8)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      74.62
_cell_measurement_theta_min      3.94
_cell_volume                     3282.44(18)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      101.27
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            70423
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'microfocus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.847
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.2673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1797 before and 0.0815 after correction.
The Ratio of minimum to maximum transmission is 0.3546.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       plank
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.101
_refine_diff_density_max         2.323
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.056(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0478P)^2^+2.6026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0680
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5923
_reflns_number_total             6011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04121g1.cif
_cod_data_source_block           1_jsop212121_a
_cod_depositor_comments
'Adding full bibliography for 7045677--7045678.cif.'
_cod_database_code               7045677
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.252
_shelx_estimated_absorpt_t_min   0.068
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.944(13)
 0.056(13)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C16)
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              34280
_olex2_submission_special_instructions 'No special instructions were received'