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_7045678
_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         'C36 H46 N2 O2 Tl2'
_chemical_formula_sum            'C36 H46 N2 O2 Tl2'
_chemical_formula_weight         947.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            16
_cell_length_a                   17.7707(5)
_cell_length_b                   25.4858(7)
_cell_length_c                   31.6358(9)
_cell_measurement_reflns_used    9548
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      74.82
_cell_measurement_theta_min      3.34
_cell_volume                     14327.9(7)
_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      100.91
_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  0.0639
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            329953
_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         68.246
_diffrn_reflns_theta_min         2.793
_diffrn_source                   'microfocus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.311
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1558 before and 0.0822 after correction.
The Ratio of minimum to maximum transmission is 0.5589.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       needle
_exptl_crystal_F_000             7264
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.574
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         13125
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0428P)^2^+27.5733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12256
_reflns_number_total             13125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04121g1.cif
_cod_data_source_block           2_jsopbca_a
_cod_depositor_comments
'Adding full bibliography for 7045677--7045678.cif.'
_cod_database_code               7045678
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.331
_shelx_estimated_absorpt_t_min   0.098
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H58-H69
 1.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C46A) = Uanis(C47A)
4. Others
 Fixed Sof: C9(0.7) H9A(0.7) H9B(0.7) H9C(0.7) C9A(0.3) H9AA(0.3) H9AB(0.3)
 H9AC(0.3) C10(0.7) H10A(0.7) H10B(0.7) H10C(0.7) C10A(0.3) H10D(0.3) H10E(0.3)
 H10F(0.3) C11(0.7) H11A(0.7) H11B(0.7) H11C(0.7) C11A(0.3) H11D(0.3) H11E(0.3)
 H11F(0.3) C46(0.8) H46A(0.8) H46B(0.8) H46C(0.8) C46A(0.2) H46D(0.2) H46E(0.2)
 H46F(0.2) C47A(0.3) H47A(0.3) H47B(0.3) H47C(0.3) C47(0.7) H47D(0.7) H47E(0.7)
 H47F(0.7)
5.a Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C10(H10A,H10B,H10C), C10A(H10D,H10E,
 H10F), C11(H11A,H11B,H11C), C11A(H11D,H11E,H11F), 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), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C46A(H46D,H46E,H46F),
 C47A(H47A,H47B,H47C), C47(H47D,H47E,H47F), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              97628
_olex2_submission_special_instructions 'No special instructions were received'