Geometric isomers of dichloridoiron(III) complexes of CTMC (5,7,12,14-tetramethyl-1,4,8,11-tetraazacyclotetradecane)
DeLancey, Stephanie S.; Clendening, Reese A.; Zeller, Matthias; Ren, Tong; Acta Crystallographica Section C 78 (2022) 507–514; doi:10.1107/S205322962200849X

data_2022657
_publ_section_title
;
 Geometric isomers of dichloridoiron(III) complexes of CTMC
 (5,7,12,14-tetramethyl-1,4,8,11-tetraazacyclotetradecane)
;
_journal_coeditor_code           LF3128
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              507
_journal_page_last               514
_journal_paper_doi               10.1107/S205322962200849X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Fe (C14 H32 N4) Cl2] Cl'
_chemical_formula_moiety         'C14 H32 Cl2 Fe N4 +, Cl -'
_chemical_formula_sum            'C14 H32 Cl3 Fe N4'
_chemical_formula_weight         418.63
_chemical_name_systematic
'<i>cis</i>-Dichlorido[(5<i>SR</i>,7<i>RS</i>,12<i>SR</i>,14<i>RS</i>)-5,7,12,14-tetramethyl-1,4,8,11-tetraazacyclotetradecane]iron(III) chloride'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2912(12)
_cell_length_b                   11.9579(19)
_cell_length_c                   17.267(3)
_cell_measurement_reflns_used    2788
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.2188
_cell_measurement_theta_min      6.5556
_cell_volume                     1918.4(5)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
APEX3 (Bruker, 2019)
;
_computing_data_reduction
;
SAINT (Bruker, 2019)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b) and
SHELXLE (H\"ubschle <i>et al.</i>, 2011)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14150
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.642
_diffrn_reflns_theta_min         6.555
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    10.153
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.5264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.948
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2055
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0894P)^2^+2.1112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                1324
_reflns_number_total             2055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3128sup1.cif
_cod_data_source_block           2
_cod_database_code               2022657
_shelx_estimated_absorpt_t_min   0.375
_shelx_estimated_absorpt_t_max   0.631
_shelx_hkl_checksum              7053
_shelx_res_checksum              99452
_cod_database_fobs_code 2022657