Syntheses, Structures and Solid-State Properties of MMX Mixed-Valence Chains, [NiII/III2(RCS2)4I]∞(R = Et,n-Pr andn-Bu): Evidence of a Spin-Peierls Transition
Minoru Mitsumi; Yuji Yoshida; Akihisa Kohyama; Yasutaka Kitagawa; Yoshiki Ozawa; Mototada Kobayashi; Koshiro Toriumi; Makoto Tadokoro; Naoshi Ikeda; Mitsutaka Okumura; Mohamedally Kurmoo; Inorganic Chemistry 48 (2009) 6680–6691; doi:10.1021/ic900630a

data_4302715
_publ_contact_author_address
; 
Department of Material Science
Graduate School of Material Science
University of Hyogo
3-2-1 Kouto, Kamigori-cho, Ako-gun, Hyogo 678-1297, Japan 
;
_publ_contact_author_email       mitsumi@sci.u-hyogo.ac.jp
_publ_contact_author_fax         +81-791-58-0154
_publ_contact_author_name        'Mitsumi, Minoru'
_publ_contact_author_phone       +81-791-58-0153
_publ_section_title
;
Syntheses, Structures and Solid-State Properties of MMX Mixed-Valence
Chains, [NiII/III2(RCS2)4I]\\infty (R = Et,n-Pr andn-Bu): Evidence of a
Spin-Peierls Transition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6680
_journal_page_last               6691
_journal_paper_doi               10.1021/ic900630a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C16 H28 I Ni2 S8'
_chemical_formula_sum            'C16 H28 I Ni2 S8'
_chemical_formula_weight         721.22
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 136.4426(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   17.7659(5)
_cell_length_b                   25.1099(8)
_cell_length_c                   13.0451(5)
_cell_measurement_reflns_used    22287
_cell_measurement_temperature    240(1)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.1
_cell_volume                     4010.1(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (A. Altomare, 1999)'
_diffrn_ambient_temperature      240(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22908
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    3.191
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2166
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.634
_refine_diff_density_min         -2.104
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         5976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+4.0010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                4546
_reflns_number_total             5976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900630a_si_002.cif
_cod_data_source_block           '[Pt2(n-PrCS2)4I]_240K'
_cod_original_cell_volume        4010.0(2)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4302715