A solid-state phase transition at 41 K involving the cooperative ordering of a fluxional pseudo-Jahn–Teller CuII system
Leech, Michael A.; Howard, Judith A. K.; Dahaoui, Slimane; Solanki, Nayan K.; Halcrow, Malcolm A.; Chemical Communications  (1999) 2245–; doi:10.1039/a906876g

data_7115191
_publ_section_title
;
 A solid-state phase transition at 41 K involving the cooperative ordering
 of a fluxional pseudo-Jahn--Teller CuII system
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2245
_journal_paper_doi               10.1039/a906876g
_journal_year                    1999
_chemical_formula_moiety         'C22 H18 Cu N10, 2 (B F4)'
_chemical_formula_sum            'C22 H18 B2 Cu F8 N10'
_chemical_formula_weight         659.62
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 97.2050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   8.4047(6)
_cell_length_b                   25.3897(18)
_cell_length_c                   18.6676(13)
_cell_measurement_reflns_used    967
_cell_measurement_temperature    31.5(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      16.37
_cell_volume                     3952.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      31.5(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'Bruker SMART-CCD'
_diffrn_measurement_method       \f-scan
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23287
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         3.39
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1986
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.549(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         9396
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.6235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                8835
_reflns_number_total             9396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            906876g.txt
_cod_data_source_block           31K
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7115191