Synthesis and structural characterization of four dichloridobis(cyclopropylalkynylamidine)metal complexes
Wang, Sida; Liebing, Phil; Engelhardt, Felix; Hilfert, Liane; Busse, Sabine; Edelmann, Frank T.; Acta Crystallographica Section E 74 (2018) 1658–1664; doi:10.1107/S2056989018014895

data_2242697
_publ_section_title
;
 Synthesis and structural characterization of four
 dichloridobis(cyclopropylalkynylamidine)metal complexes
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1658
_journal_page_last               1664
_journal_paper_doi               10.1107/S2056989018014895
_journal_volume                  74
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Fe Cl2 (C12 H20 N2)2]'
_chemical_formula_moiety         'C24 H40 Cl2 Fe N4'
_chemical_formula_sum            'C24 H40 Cl2 Fe N4'
_chemical_formula_weight         511.35
_chemical_name_systematic
Dichloridobis(3-cyclopropyl-<i>N</i>,<i>N</i>'-diisopropylprop-2-ynamidine)iron(II)
_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     dual
_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                   17.5703(9)
_cell_length_b                   30.9167(12)
_cell_length_c                   10.1110(6)
_cell_measurement_reflns_used    5377
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.987
_cell_measurement_theta_min      2.416
_cell_volume                     5492.5(5)
_computing_cell_refinement
;
X-Area (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-Area and X-Red (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
Diamond (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5377
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.987
_diffrn_reflns_theta_min         2.416
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.8876
_exptl_absorpt_correction_T_min  0.8366
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
X-Area and X-Red (Stoe & Cie, 2002)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.423
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 846 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2495
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0450P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0741
_reflns_number_gt                2239
_reflns_number_total             2495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2740sup1.cif
_cod_data_source_block           4
_cod_database_code               2242697
_shelx_estimated_absorpt_t_min   0.821
_shelx_estimated_absorpt_t_max   0.833
_shelx_hkl_checksum              33333
_shelx_res_checksum              55037
_cod_database_fobs_code 2242697