Water-controlled synthesis and single-crystal structural transformations of a cyanide-bridged W(IV)-Ni(II) molecular wheel complex and 3D networks
Dao-Peng Zhang; Li-Fang Zhang; Guo-Ling Li; Zhong-Hai Ni; Chem.Commun. 49 (2013) 9582–; doi:10.1039/c3cc46063k

data_7109873
_publ_section_title
;
 Water-controlled synthesis and single-crystal structural transformations
 of a cyanide-bridged W(IV)-Ni(II) molecular wheel complex and 3D networks
;
_journal_name_full               Chem.Commun.
_journal_page_first              9582
_journal_paper_doi               10.1039/c3cc46063k
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C228 H352 N96 Ni12 O42 W6'
_chemical_formula_weight         6917.68
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   33.5208(19)
_cell_length_b                   33.5208(19)
_cell_length_c                   24.994(3)
_cell_measurement_reflns_used    2871
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.861
_cell_measurement_theta_min      2.761
_cell_volume                     24322(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40039
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    2.868
_exptl_absorpt_correction_T_max  0.7068
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             10524
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9484
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+88.1983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                7298
_reflns_number_total             9484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46063k.txt
_cod_data_source_block           1
_cod_original_cell_volume        24322(3)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7109873