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_7712624
_publ_section_title
;
 Trimethyltriazacyclohexane Coordination Chemistry of Simple Rare-Earth
 Metal Salts
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00242J
_journal_year                    2023
_chemical_formula_sum            'C13 H29 I3 La N3 O'
_chemical_formula_weight         763.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-01-16 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0712(13)
_cell_length_b                   10.0909(8)
_cell_length_c                   13.2624(10)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.40
_cell_measurement_theta_min      2.38
_cell_volume                     2150.8(3)
_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      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25962
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.510
_diffrn_reflns_theta_min         2.383
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.295
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.356
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.082
_refine_diff_density_max         3.879
_refine_diff_density_min         -1.764
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details
; 
 Refined as a perfect inversion twin. 
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         6364
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+8.2419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5660
_reflns_number_total             6364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00242j2.cif
_cod_data_source_block           jcw114
_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 
;
_cod_database_code               7712624
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.390
_shelx_estimated_absorpt_t_max   0.626
_exptl_absorpt_special_details
; 
Reflections not merged 
27344 Corrected reflections written to file jcw114s.hkl 
Estimated minimum and maximum transmission:  0.3064  0.4330 
The ratio (0.7076) of these values is more reliable than their absolute values! 
Additional spherical absorption correction applied with mu*r =  0.6000 
Lambda/2 correction factor = 0.00150 
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_shelx_res_checksum              15071