Trimethyltriazacyclohexane Coordination Chemistry of Simple Rare-Earth Metal Salts
Wedal, Justin C.; Ziller, Joseph W.; Evans, William J.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00242J

data_7712622
_publ_section_title
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 Trimethyltriazacyclohexane Coordination Chemistry of Simple Rare-Earth
 Metal Salts
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00242J
_journal_year                    2023
_chemical_formula_moiety         'C12 H30 Cl3 La N6'
_chemical_formula_sum            'C12 H30 Cl3 La N6'
_chemical_formula_weight         503.67
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-03-10 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   11.9427(7)
_cell_length_b                   11.9427(7)
_cell_length_c                   10.5184(6)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.76
_cell_volume                     1299.23(13)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART 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  0.0510
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            31987
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.502
_diffrn_reflns_theta_min         2.762
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6149
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         1382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0124
_refine_ls_R_factor_gt           0.0118
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+0.2881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0315
_refine_ls_wR_factor_ref         0.0317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1329
_reflns_number_total             1382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00242j2.cif
_cod_data_source_block           jcw84
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
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_cod_original_cell_volume        1299.23(17)
_cod_database_code               7712622
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.523
_shelx_estimated_absorpt_t_max   0.750
_exptl_absorpt_special_details
; 
Reflections not merged 
32254 Corrected reflections written to file jcw84s.hkl 
Estimated minimum and maximum transmission:  0.6149  0.7461 
The ratio (0.8242) of these values is more reliable than their absolute values! 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
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_shelx_res_checksum              89463
_shelx_fab_checksum              37750