Chiral (LH)2L2Cu3 Trinuclear Paramagnetic Nodes in Octacyanidometalate-Bridged Helical Chains.
Stefańczyk, Olaf; Rams, Michał; Majcher, Anna M.; Mathonière, Corine; Sieklucka, Barbara; Inorganic chemistry 53 (2014) 3874–; doi:10.1021/ic500271f

data_4337889
_publ_section_title
;
 Chiral (LH)2L2Cu3 Trinuclear Paramagnetic Nodes in
 Octacyanidometalate-Bridged Helical Chains.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3874
_journal_paper_doi               10.1021/ic500271f
_journal_volume                  53
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H38 Cu3 N16 O4 W, H2 O'
_chemical_formula_sum            'C20 H40 Cu3 N16 O5 W'
_chemical_formula_weight         959.17
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-17T15:14:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2460(2)
_cell_length_b                   17.5290(2)
_cell_length_c                   20.6140(4)
_cell_measurement_reflns_used    7741
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6231.72(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.325765E-1
_diffrn_orient_matrix_UB_12      -0.437782E-1
_diffrn_orient_matrix_UB_13      0.149882E-1
_diffrn_orient_matrix_UB_21      -0.35648E-1
_diffrn_orient_matrix_UB_22      -0.78382E-2
_diffrn_orient_matrix_UB_23      0.37676E-1
_diffrn_orient_matrix_UB_31      -0.320972E-1
_diffrn_orient_matrix_UB_32      -0.357266E-1
_diffrn_orient_matrix_UB_33      -0.266319E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13556
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.77
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.760
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.78
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+8.4796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                6563
_reflns_number_total             7101
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic500271f_si_003.cif
_cod_data_source_block           CubdapW
_cod_depositor_comments
'Adding full bibliography for 4337888--4337889.cif.'
_cod_database_code               4337889