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_2021355
_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)2 (C4 H8 O1)2]'
_chemical_formula_moiety         'C48 H52 Fe N6 O2'
_chemical_formula_sum            'C48 H52 Fe N6 O2'
_chemical_formula_weight         800.80
_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-\k<i>N</i>^7^)bis(tetrahydrofuran-\k<i>O</i>)iron(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9624(12)
_cell_length_b                   15.8047(11)
_cell_length_c                   32.747(2)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.7258
_cell_measurement_theta_min      3.8675
_cell_volume                     8261.4(10)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker X8 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  0.0546
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23792
_diffrn_reflns_theta_full        66.721
_diffrn_reflns_theta_max         66.721
_diffrn_reflns_theta_min         3.867
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    3.292
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(APEX2; Bruker, 2014)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         7194
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0545P)^2^+1.2424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                5411
_reflns_number_total             7194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qs3077sup1.cif
_cod_data_source_block           10
_cod_original_cell_volume        8261.5(10)
_cod_database_code               2021355
_cod_database_fobs_code          2021355
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.827
_shelx_hkl_checksum              59451
_shelx_res_checksum              82403