Unsymmetrical Linear Pentanuclear Nickel String Complexes: [Ni5(tpda)4(H2O)(BF4)](BF4)2 and [Ni5(tpda)4(SO3CF3)2](SO3CF3)
Chen-Yu Yeh; Yi-Li Chiang; Gene-Hsiang Lee; Shie-Ming Peng; Inorganic Chemistry 41 (2002) 4096–4098; doi:10.1021/ic025582v

data_4318339
_publ_contact_author
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Shie-Ming Peng
Department of Chemistry, National Taiwan University, Taipei, Taiwan
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_publ_contact_author_email       smpeng@mail.ch.ntu.edu.tw
_publ_section_title
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 Unsymmetrical Linear Pentanuclear Nickel String Complexes:
 [Ni5(tpda)4(H2O)(BF4)](BF4)2 and [Ni5(tpda)4(SO3CF3)2](SO3CF3)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4096
_journal_page_last               4098
_journal_paper_doi               10.1021/ic025582v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C64 H54 B3 Cl8 F12 N20 Ni5 O'
_chemical_formula_weight         1956.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 92.2425(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3022(1)
_cell_length_b                   31.0705(3)
_cell_length_c                   15.8109(2)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.45
_cell_volume                     7511.49(13)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_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  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52924
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3940
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.414
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.373
_refine_ls_extinction_coef       0.0076(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         17219
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1417P)^2^+25.2340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2188
_refine_ls_wR_factor_ref         0.2640
_reflns_number_gt                10575
_reflns_number_total             17219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025582v_s1_1.cif
_cod_data_source_block           '[Ni5(tpda)4(H2O)(BF4)](BF4)2(compound1)'
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4318339