A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended with Hydrogen-Bond Donor/Acceptor Groups
Stéphane A. Baudron; Narcis Avarvari; Patrick Batail; Inorganic Chemistry 44 (2005) 3380–3382; doi:10.1021/ic050174n

data_1100744
_publ_contact_author
; Dr Patrick Batail 

  Laboratoire Chimie Ing\'enierie Mol\'eculaires et

  Mat\'eriaux d'Angers,

  UMR 6200 CNRS-Universit\'e d'Angers,

  Bat. K, 2, Boulevard Lavoisier, Angers, France 

;
_publ_contact_author_email       patrick.batail@univ-angers.fr
_publ_contact_author_fax         '33 2 41 73 50 11'
_publ_contact_author_phone       '33 2 41 73 52 64'
_publ_section_title
;

A Straightforward Synthesis of Diverse Nickel Dithiolene Complexes Appended

with Hydrogen-Bond Donor/Acceptor Groups

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3380
_journal_page_last               3382
_journal_paper_doi               10.1021/ic050174n
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H76 N6 Ni O2 S4'
_chemical_formula_weight         860.02
_chemical_name_common            (n-Bu4N)[Ni(mant)2]
_chemical_name_systematic
;

 ?

;
_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                70.09(3)
_cell_angle_beta                 77.79(2)
_cell_angle_gamma                76.68(3)
_cell_formula_units_Z            1
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_cell_length_b                   11.804(3)
_cell_length_c                   12.478(3)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      2.1
_cell_volume                     1216.7(5)
_computing_cell_refinement       'SELECT, 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, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi. incr. = 1.9'
_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  0.1174
_diffrn_reflns_av_sigmaI/netI    0.2538
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
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_diffrn_reflns_number            12471
_diffrn_reflns_theta_full        26.23
_diffrn_reflns_theta_max         26.23
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_correction_T_min  0.9061
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, STOE-IPDS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       platelet
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.2694
_exptl_crystal_size_mid          0.1156
_exptl_crystal_size_min          0.0230
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.592
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.592
_refine_ls_R_factor_all          0.1528
_refine_ls_R_factor_gt           0.0414
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                1579
_reflns_number_total             4462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050174nsi20050201_114543.cif
_cod_data_source_block           sb687e
_cod_original_cell_volume        1216.6(4)
_cod_database_code               1100744