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_2022655
_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] [Fe Cl4]'
_chemical_formula_moiety         'C14 H32 Cl2 Fe N4 +, Cl4 Fe -'
_chemical_formula_sum            'C14 H32 Cl6 Fe2 N4'
_chemical_formula_weight         580.83
_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)
tetrachloridoferrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 100.452(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3512(13)
_cell_length_b                   6.4815(4)
_cell_length_c                   18.0490(10)
_cell_measurement_reflns_used    9346
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.0757
_cell_measurement_theta_min      3.3040
_cell_volume                     2341.3(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            71685
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.205
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.480
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         4483
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0297P)^2^+1.6800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                3561
_reflns_number_total             4483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lf3128sup1.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2022655
_shelx_estimated_absorpt_t_min   0.699
_shelx_estimated_absorpt_t_max   0.699
_shelx_hkl_checksum              86137
_shelx_res_checksum              41906
_cod_database_fobs_code 2022655