Structural phase transition due to the flexible supramolecule of (4-cyanomethylanilinium)([18]crown-6) in [Ni(dmit)2]− crystal
Ye, Qiong; Akutagawa, Tomoyuki; Ye, Heng-Yun; Hang, Tian; Ge, Jia-Zhen; Xiong, Ren-Gen; Noro, Shin-ichiro; Nakamura, Takayoshi; CrystEngComm 13 (2011) 6185–; doi:10.1039/c1ce05581j

data_7215410
_publ_section_title
;
 Structural phase transition due to the flexible supramolecule of
 (4-cyanomethylanilinium)([18]crown-6) in [Ni(dmit)2]&#x2212; crystal
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6185
_journal_paper_doi               10.1039/c1ce05581j
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C26 H31 N2 Ni O6 S10'
_chemical_formula_weight         846.84
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   16.075(3)
_cell_length_b                   25.415(4)
_cell_length_c                   35.366(5)
_cell_measurement_temperature    100
_cell_volume                     14449(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1195
_diffrn_reflns_av_sigmaI/netI    0.1222
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            122762
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.156
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6992.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.811
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.608(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1623
_refine_ls_number_reflns         32341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                18764
_reflns_number_total             32341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05581j.txt
_cod_data_source_block           shelxl
_cod_original_cell_volume        14448(4)
_cod_database_code               7215410