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_2021796
_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_formula_iupac          '[Fe Cl2 (C16 H36 N4)] [Fe Cl4]'
_chemical_formula_moiety         'C16 H36 Cl2 Fe N4 +, Cl4 Fe -'
_chemical_formula_sum            'C16 H36 Cl6 Fe2 N4'
_chemical_formula_weight         608.89
_chemical_name_systematic
;
Dichlorido(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)iron(III)
tetrachloridoferrate
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 95.3558(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5569(2)
_cell_length_b                   19.1663(5)
_cell_length_c                   20.2946(5)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      80.2194
_cell_measurement_theta_min      3.1759
_cell_volume                     2539.32(12)
_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 7.4074
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS'
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26483
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         81.308
_diffrn_reflns_theta_min         3.178
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    15.058
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.4258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.569
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5481
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0331P)^2^+2.0722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                4930
_reflns_number_total             5481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cu3157sup1.cif
_cod_data_source_block           2
_cod_database_code               2021796
_shelx_estimated_absorpt_t_min   0.172
_shelx_estimated_absorpt_t_max   0.520
_shelx_hkl_checksum              51176
_shelx_res_checksum              61502
_cod_database_fobs_code 2021796