Formation and structure of the first metal complexes comprising amidinoguanidinate ligands
Sroor, Farid M.; Liebing, Phil; Hrib, Cristian G.; Gräsing, Daniel; Hilfert, Liane; Edelmann, Frank T.; Acta Crystallographica Section E 72 (2016) 1526–1531; doi:10.1107/S2056989016015322

data_2241870
_publ_section_title
;
 Formation and structure of the first metal complexes comprising
 amidinoguanidinate ligands
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1526
_journal_page_last               1531
_journal_paper_doi               10.1107/S2056989016015322
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Li Ho Cl2 (C4 H8 O)2 (C17 H31 N2) (C30 H53 N4)]'
_chemical_formula_moiety         'C55 H100 Cl2 Ho Li N6 O2'
_chemical_formula_sum            'C55 H100 Cl2 Ho Li N6 O2'
_chemical_formula_weight         1120.17
_chemical_name_systematic
'[Bis(tetrahydrofuran)lithium]-di-\m-chlorido-{(<i>N</i>,<i>N</i>'-dicyclohexyl-1-butylamidinato-\k^2^<i>N</i>^1^,<i>N</i>^2^)[<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>'''-tetracyclohexyl-1-(1-butylamidinato)guanidinato-\k^2^<i>N</i>^1^,<i>N</i>^2^]holmate(III)}'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
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_cell_angle_beta                 97.20(3)
_cell_angle_gamma                109.50(3)
_cell_formula_units_Z            2
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_cell_length_b                   15.095(3)
_cell_length_c                   16.786(3)
_cell_measurement_reflns_used    29309
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      2.19
_cell_volume                     2967.5(13)
_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
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0776
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.320
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
(X-AREA and X-RED; Stoe & Cie, 2002)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_exptl_crystal_size_rad          0.13
_refine_diff_density_max         0.984
_refine_diff_density_min         -1.682
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     552
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0158P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                9625
_reflns_number_total             12948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2679sup1.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        2967.5(12)
_cod_database_code               2241870
_shelx_estimated_absorpt_t_min   0.636
_shelx_estimated_absorpt_t_max   0.844
_shelx_hkl_checksum              84357
_shelx_res_checksum              67791
_cod_database_fobs_code 2241870