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_4505748
_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_formula_moiety         '(C3 H10 N)2, C8 N4 S4 Ni'
_chemical_formula_sum            'C14 H20 N6 Ni S4'
_chemical_formula_weight         459.31
_chemical_name_common            '(HNMe3)2, Ni(mnt)2'
_chemical_name_systematic
; 
Bis(trimethylammonium), bis(dicyanoethylene-1,2-dithiolato)nickelate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                64.74(2)
_cell_angle_beta                 70.307(16)
_cell_angle_gamma                89.487(15)
_cell_formula_units_Z            1
_cell_length_a                   7.4343(13)
_cell_length_b                   8.6973(15)
_cell_length_c                   9.772(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.17
_cell_measurement_theta_min      2.60
_cell_volume                     531.2(2)
_computing_cell_refinement       'Enraf-Nonius Mach3'
_computing_data_collection       'Enraf-Nonius MACH3'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Enraf-Nonius Mach3'
_diffrn_measurement_method       'omega/2 theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2126
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  0.95580
_exptl_absorpt_correction_T_min  0.92073
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
psi-scan from reflections with chi close to
90 deg.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             238
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.4702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                1276
_reflns_number_total             1965
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0340805si20030519_093723.cif
_cod_data_source_block           sd1abs
_cod_original_cell_volume        531.23(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505748