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_2241869
_publ_section_title
;
 Formation and structure of the first metal complexes comprising
 amidinoguanidinate ligands
;
_journal_coeditor_code           ZL2679
_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          '[Li2 C18 H37 N4)2 (C4 H8 O)2]'
_chemical_formula_moiety         'C44 H90 Li2 N8 O2'
_chemical_formula_sum            'C44 H90 Li2 N8 O2'
_chemical_formula_weight         777.11
_chemical_name_systematic
Bis[\m-<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>'''-tetraisopropyl-1-(1-butylamidinato)guanidinato-\k^3^<i>N</i>^1^,<i>N</i>^2^:<i>N</i>^2^]bis[(tetrahydrofuran)lithium]
_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-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 92.8380(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.93297(7)
_cell_length_b                   13.72390(10)
_cell_length_c                   18.07940(13)
_cell_measurement_reflns_used    18888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6226
_cell_measurement_theta_min      3.2175
_cell_volume                     2461.54(3)
_computing_cell_refinement
;
CrysAlisPro (Agilent, 2011)
;
_computing_data_collection
;
CrysAlisPro (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlisPro (Agilent, 2011)
;
_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      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Agilent Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30246
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.809
_diffrn_reflns_theta_min         4.046
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent, 2011)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.205
_refine_ls_extinction_coef       0.00067(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0474P)^2^+0.6355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                4657
_reflns_number_total             5126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2679sup1.cif
_cod_data_source_block           compound_2
_cod_database_code               2241869
_cod_database_fobs_code          2241869
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.981
_shelx_hkl_checksum              94000
_shelx_res_checksum              85665