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_2242698
_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_formula_iupac          '[Fe Cl2 (C18 H28 N2)2]'
_chemical_formula_moiety         'C36 H56 Cl2 Fe N4'
_chemical_formula_sum            'C36 H56 Cl2 Fe N4'
_chemical_formula_weight         671.59
_chemical_name_systematic
Dichloridobis(<i>N</i>,<i>N</i>'-dicyclohexyl-3-cyclopropylprop-2-ynamidine)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   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.24(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.905(7)
_cell_length_b                   12.500(6)
_cell_length_c                   20.742(11)
_cell_measurement_reflns_used    17648
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.349
_cell_measurement_theta_min      1.903
_cell_volume                     3602(3)
_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      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.903
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_T_max  0.9078
_exptl_absorpt_correction_T_min  0.8383
_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    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.327
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7036
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0293P)^2^+1.8416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                6355
_reflns_number_total             7036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2740sup1.cif
_cod_data_source_block           5
_cod_original_cell_volume        3603(3)
_cod_database_code               2242698
_shelx_estimated_absorpt_t_min   0.860
_shelx_estimated_absorpt_t_max   0.932
_shelx_hkl_checksum              82706
_shelx_res_checksum              71501
_cod_database_fobs_code 2242698