Iron(II) complexes of dimethyltriazacyclophane
Lee, Wei-Tsung; Zeller, Matthias; Upp, David; Politanska, Yuliya; Steinman, Doug; Al-Assil, Talal; Becker, Daniel P.; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618015255

data_2021354
_publ_section_title
;
 Iron(II) complexes of dimethyltriazacyclophane
;
_journal_coeditor_code           QS3077
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618015255
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Fe (C20 H18 N3)4]'
_chemical_formula_moiety         'C80 H72 Fe2 N12'
_chemical_formula_sum            'C80 H72 Fe2 N12'
_chemical_formula_weight         1313.19
_chemical_name_systematic
;Bis(\m-1,4-dimethyltribenzo[<i>b</i>,<i>e</i>,<i>h</i>][1,4,7]triazacyclonona-2,5,8-trien-7-ido)-1:2\k^2^<i>N</i>^1^,<i>N</i>^7^:\k<i>N</i>^7^;
1:2\k<i>N</i>^7^:\k^2^<i>N</i>^7^,<i>C</i>^6^-bis[(\m-1,4-dimethyltribenzo[<i>b</i>,<i>e</i>,<i>h</i>][1,4,7]triazacyclonona-2,5,8-trien-7-ido-\k<i>N</i>^7^)iron(II)]
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.191(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.758(2)
_cell_length_b                   12.7682(13)
_cell_length_c                   31.382(3)
_cell_measurement_reflns_used    8887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.7534
_cell_measurement_theta_min      2.9820
_cell_volume                     8233.8(14)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and
SHELXLE (H\"ubschle <i>et al.</i>, 2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker Prospector CCD'
_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  0.1333
_diffrn_reflns_av_unetI/netI     0.1099
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52565
_diffrn_reflns_theta_full        66.901
_diffrn_reflns_theta_max         66.901
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.4784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>APEX2</i>; Bruker, 2014)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       rod
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.544
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         14191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.0761
_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^)+(0.0816P)^2^+5.4245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1927
_reflns_number_gt                8827
_reflns_number_total             14191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qs3077sup1.cif
_cod_data_source_block           9
_cod_original_cell_volume        8233.7(14)
_cod_database_code               2021354
_cod_database_fobs_code          2021354
_shelx_estimated_absorpt_t_min   0.722
_shelx_estimated_absorpt_t_max   0.857
_shelx_hkl_checksum              15717
_shelx_res_checksum              30621
_shelx_fab_checksum              14357