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_2022656
_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, C H4 O'
_chemical_formula_moiety         'C14 H32 Cl2 Fe N4 +, Cl -, C H4 O'
_chemical_formula_sum            'C15 H36 Cl3 Fe N4 O'
_chemical_formula_weight         450.68
_chemical_name_systematic
;<i>trans</i>-Dichlorido[(5<i>SR</i>,7<i>RS</i>,12<i>RS</i>,14<i>SR</i>)-4,7,12,14-tetramethyl-1,4,8,11-tetraazacyclotetradecane]iron(III)
chloride methanol monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 95.024(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1632(4)
_cell_length_b                   20.8470(12)
_cell_length_c                   12.1387(7)
_cell_measurement_reflns_used    9046
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.0931
_cell_measurement_theta_min      2.5799
_cell_volume                     2057.8(2)
_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
;
SHELXT2014 (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 0.998
_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  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            125711
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.158
_diffrn_reflns_theta_min         2.689
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6787
_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    1.455
_exptl_crystal_description       Needle
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.576
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         7859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0258P)^2^+0.6993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0608
_reflns_number_gt                6505
_reflns_number_total             7859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3128sup1.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022656
_shelx_estimated_absorpt_t_min   0.699
_shelx_estimated_absorpt_t_max   0.905
_shelx_hkl_checksum              44032
_shelx_res_checksum              98010
_cod_database_fobs_code 2022656