Cu(i)/(ii) based catalytic ionic liquids, their metallo-laminate solid state structures and catalytic activities in oxidative methanol carbonylation
Stricker, Marion; Linder, Thomas; Oelkers, Benjamin; Sundermeyer, Jörg; Green Chemistry 12 (2010) 1589–; doi:10.1039/c003948a

data_7212701
_publ_section_title
;
 Cu(i)/(ii) based catalytic ionic liquids, their metallo-laminate solid
 state structures and catalytic activities in oxidative methanol
 carbonylation
;
_journal_issue                   9
_journal_name_full               'Green Chemistry'
_journal_page_first              1589
_journal_paper_doi               10.1039/c003948a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         '4(C16 H31 N2), Br8 Cu4'
_chemical_formula_sum            'C64 H124 Br8 Cu4 N8'
_chemical_formula_weight         1899.15
_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                73.875(17)
_cell_angle_beta                 87.515(17)
_cell_angle_gamma                87.742(17)
_cell_formula_units_Z            2
_cell_length_a                   10.3068(13)
_cell_length_b                   16.172(2)
_cell_length_c                   25.595(4)
_cell_measurement_reflns_used    6115
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.65
_cell_measurement_theta_min      2.35
_cell_volume                     4092.9(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2262
_diffrn_reflns_av_sigmaI/netI    0.4514
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40859
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    4.969
_exptl_absorpt_correction_T_max  0.5082
_exptl_absorpt_correction_T_min  0.4021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.604
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         14954
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      0.603
_refine_ls_R_factor_all          0.2416
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                3090
_reflns_number_total             14954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c003948a.txt
_cod_data_source_block           msc03b
_cod_original_cell_volume        4093.0(10)
_cod_database_code               7212701