Flexibility of cubane-like Cu4I4 framework: temperature dependence of molecular structure and luminescence thermochromism of [Cu4I4(PPh3)4] in two polymorphic crystalline states.
Kitagawa, Hakuba; Ozawa, Yoshiki; Toriumi, Koshiro; Chemical communications (Cambridge, England) 46 (2010) 6302–6304; doi:10.1039/c0cc01434f

data_7113007
_publ_section_title
;
 Flexibility of cubane-like Cu4I4 framework: temperature dependence of
 molecular structure and luminescence thermochromism of [Cu4I4(PPh3)4] in
 two polymorphic crystalline states.
;
_journal_issue                   34
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6302
_journal_page_last               6304
_journal_paper_doi               10.1039/c0cc01434f
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         '((C6 H5)3 P) Cu I)4'
_chemical_formula_sum            'C72 H60 Cu4 I4 P4'
_chemical_formula_weight         1810.84
_chemical_name_systematic
tetrakis(triphenylphosphane-\m~3~-iodo-copper(I))
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.305(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4031(3)
_cell_length_b                   26.3883(5)
_cell_length_c                   19.3872(14)
_cell_measurement_temperature    77(1)
_cell_volume                     6766.7(5)
_computing_cell_refinement       'R-AXIS (Rigaku Co. Ltd., 2008)'
_computing_data_collection       'R-AXIS (Rigaku Co. Ltd., 2008)'
_computing_data_reduction
'RAPID-AUTO (Rigaku Co. Ltd., 2008), SORTAV (Blessing, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      77(1)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'SPring-8 BL02B1 Large cylindrical Image-Plate camera'
_diffrn_measurement_method       '\w axis oscillation'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.5886
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            110090
_diffrn_reflns_theta_full        24.49
_diffrn_reflns_theta_max         24.49
_diffrn_reflns_theta_min         1.28
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_diffrn_source_type              'SPring-8 beamline BL02B1'
_exptl_absorpt_coefficient_mu    1.84
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.8407
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Higashi, Rigaku Co.Ltd., 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3520
_exptl_crystal_recrystallization_method chloroform/ether
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.749
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         19775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.749
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0178
_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^)+(0.0106P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0312
_refine_ls_wR_factor_ref         0.0315
_reflns_number_gt                14623
_reflns_number_total             19775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01434f.txt
_cod_data_source_block           cuipph_mono_077k
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7113007