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_4505750
_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         'C5 H6 N, C8 N4 Ni S4'
_chemical_formula_sum            'C13 H6 N5 Ni S4'
_chemical_formula_weight         419.18
_chemical_name_common            'PyH, Ni(mnt)2'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.047(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5462(15)
_cell_length_b                   6.3851(3)
_cell_length_c                   17.4351(16)
_cell_measurement_reflns_used    6589
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.35
_cell_volume                     1625.7(3)
_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, Stoe-IPDS'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       'oscillation, phi incr. 1.3 deg.'
_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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12093
_diffrn_reflns_theta_full        25.76
_diffrn_reflns_theta_max         25.76
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_correction_T_min  0.7559
_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    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                2040
_reflns_number_total             3013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg0340805si20030519_093723.cif
_cod_data_source_block           mf279a
_cod_original_cell_volume        1625.7(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4505750