Bifurcated Hydrogen Bonds as a Key Feature in the Solid State Organization of Paramagnetic Dithiolene Complexes
Fourmigué, Marc; Mézière, Cécile; Dolou, Sébastien; Crystal Growth & Design 3 (2003) 805–; doi:10.1021/cg0340805

data_4505749
_publ_section_title
;
 Bifurcated Hydrogen Bonds as a Key Feature in the Solid State
 Organization of Paramagnetic Dithiolene Complexes
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              805
_journal_paper_doi               10.1021/cg0340805
_journal_volume                  3
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C8 N4 Ni S4, C3 H10 N, (C2 H6 O)0.4'
_chemical_formula_structural     'C11 H10 N5 NI S4'
_chemical_formula_sum            'C11.8 H12 N5 Ni O0.4 S4'
_chemical_formula_weight         417.21
_chemical_name_common            'HNMe3, Ni(mnt)2'
_chemical_name_systematic
;
Trimethylammonium, bis(dicyanoethylene-1,2-dithiolato)nickelate
ethanol solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2002-05-30T16:12:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.097(13)
_cell_angle_beta                 80.736(14)
_cell_angle_gamma                70.242(14)
_cell_formula_units_Z            5
_cell_length_a                   11.4302(15)
_cell_length_b                   13.7495(14)
_cell_length_c                   15.4235(17)
_cell_measurement_reflns_used    7122
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      2.05
_cell_measurement_wavelength     0.71073
_cell_volume                     2251.3(5)
_computing_cell_refinement       'CELL (Stoe -IPDS)'
_computing_data_collection       'EXPOSE (Stoe-IPDS)'
_computing_data_reduction        'INTEGRATE (Stoe-IPDS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'oscillation, phi incr. 1.2 deg.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1365
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22135
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.544
_exptl_absorpt_correction_T_max  0.7384
_exptl_absorpt_correction_T_min  0.7197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated plate'
_exptl_crystal_F_000             1065
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.681
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         8132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.681
_refine_ls_R_factor_all          0.123
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                3624
_reflns_number_total             8132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0340805si20030519_093723.cif
_cod_data_source_block           multisca
_cod_original_cell_volume        2251.3(4)
_cod_original_formula_sum        'C11.80 H12 N5 Ni O0.40 S4'
_cod_database_code               4505749