Crystal structures of two (5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)iron(III) complexes
Clendening, Reese A.; Zeller, Matthias; Ren, Tong; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619013925

data_2021795
_publ_section_title
;
 Crystal structures of two
 (5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)iron(III)
 complexes
;
_journal_coeditor_code           CU3157
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619013925
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_iupac          '[Fe Cl2 (C16 H36 N4)] Cl'
_chemical_formula_moiety         'C16 H36 Cl2 Fe N4 +, Cl -'
_chemical_formula_sum            'C16 H36 Cl3 Fe N4'
_chemical_formula_weight         446.69
_chemical_name_systematic
;
Dichlorido(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)iron(III)
chloride
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   mixed
_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            8
_cell_length_a                   34.5658(16)
_cell_length_b                   9.3832(4)
_cell_length_c                   12.5209(6)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.3886
_cell_measurement_theta_min      2.7761
_cell_volume                     4061.0(3)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015) and
SHELXLE (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXM (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17097
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.412
_diffrn_reflns_theta_min         2.776
_diffrn_source                   'sealed tube X-ray source'
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.5952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.584
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.004(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                3897
_reflns_number_total             4166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cu3157sup1.cif
_cod_data_source_block           1
_cod_database_code               2021795
_shelx_estimated_absorpt_t_min   0.821
_shelx_estimated_absorpt_t_max   0.945
_shelx_hkl_checksum              29991
_shelx_res_checksum              82934
_cod_database_fobs_code 2021795