Organometallic Trinuclear Niobium Cluster Complex in Aqueous Solution: Synthesis and Characterization of Niobium Complexes Containing Nb3(μ-η2:η2(perp.)-NCCH3)(μ2-O)36+ Cluster Core
Hans Arni Nybo Joensen; Gro Kallehave Hansson; Svetlana G. Kozlova; Artem L. Gushchin; Inger Søtofte; Bee-Lean Ooi; Inorganic Chemistry 49 (2010) 1720–1727; doi:10.1021/ic9019316

data_4314777
_publ_section_title
;
 Organometallic Trinuclear Niobium Cluster Complex in Aqueous Solution:
 Synthesis and Characterization of Niobium Complexes Containing
 Nb3(\m-\h2:\h2(perp.)-NCCH3)(\m2-O)36+ Cluster Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1720
_journal_page_last               1727
_journal_paper_doi               10.1021/ic9019316
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '((CH3)3NH)3[NB3O3(NCCH3)(NCS)9]2.5 H2O'
_chemical_formula_sum            'C20 H38 N13 Nb3 O5.5 S9'
_chemical_formula_weight         1115.90
_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                74.754(3)
_cell_angle_beta                 86.141(3)
_cell_angle_gamma                62.668(3)
_cell_formula_units_Z            2
_cell_length_a                   13.2686(18)
_cell_length_b                   13.943(2)
_cell_length_c                   17.524(2)
_cell_measurement_reflns_used    19836
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      1.21
_cell_volume                     2773.3(6)
_computing_cell_refinement       'SAINT (Bruker AXS,1998)'
_computing_data_collection       'SMART (Bruker AXS,1998)'
_computing_data_reduction        'SAINT (Bruker AXS,1998)'
_computing_molecular_graphics    'SHELXTL,ver.6.12 (Sheldrick,2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL,ver.6.12 (Sheldrick,2001)'
_computing_structure_solution    'SHELXTL,ver.6.12 (Sheldrick,2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Siemens SMART CCD Platform'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.1047
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19836
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         1.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,ver2.03 (Sheldrick,2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.727
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         12327
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.0933
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1712P)^2^+5.6066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2582
_refine_ls_wR_factor_ref         0.3041
_reflns_number_gt                7125
_reflns_number_total             12327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9019316_si_002.cif
_cod_data_source_block           nbp
_cod_original_cell_volume        2773.4(7)
_cod_original_formula_sum        'C20 H38 N13 Nb3 O5.50 S9'
_cod_database_code               4314777