Ligand dependent topology and spontaneous resolution in high-spin cyano-bridged Ni3W2 clusters.
Nowicka, Beata; Reczyński, Mateusz; Rams, Michał; Wasiutyński, Tadeusz; Nitek, Wojciech; Sieklucka, Barbara; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12423–12431; doi:10.1039/c6dt02119k

data_7039787
_publ_section_title
;
 Ligand dependent topology and spontaneous resolution in high-spin
 cyano-bridged Ni3W2 clusters.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12423
_journal_page_last               12431
_journal_paper_doi               10.1039/c6dt02119k
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C88 H96 N28 Ni3 O24 W2'
_chemical_formula_sum            'C88 H96 N28 Ni3 O24 W2'
_chemical_formula_weight         2473.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-04-18T10:55:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-01-12 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   20.844(5)
_cell_length_b                   22.424(5)
_cell_length_c                   24.033(5)
_cell_measurement_reflns_used    24679
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     11233(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0378166
_diffrn_orient_matrix_UB_12      0.0156669
_diffrn_orient_matrix_UB_13      0.0250219
_diffrn_orient_matrix_UB_21      -0.0241007
_diffrn_orient_matrix_UB_22      -0.034457
_diffrn_orient_matrix_UB_23      -0.0148499
_diffrn_orient_matrix_UB_31      0.0122434
_diffrn_orient_matrix_UB_32      -0.0226502
_diffrn_orient_matrix_UB_33      0.0326859
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_unetI/netI     0.057
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59108
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.97
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    2.611
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       prism
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         24965
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+3.8399P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                20184
_reflns_number_total             24965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02119k2.cif
_cod_data_source_block           msniw1
_cod_depositor_comments
'Adding full bibliography for 7039785--7039787.cif.'
_cod_database_code               7039787
_shelxl_version_number           2012-9
_shelx_res_checksum              40845