(Acetylacetonato-κ^2^<i>O</i>,<i>O</i>')chloridotrimethanolatoniobium(V)
Herbst, Leandra; Koen, Renier; Roodt, Andreas; Visser, Hendrik G.; Acta Crystallographica Section E 66 (2010) m801–m802; doi:10.1107/S1600536810021719

data_2226633
_publ_section_title
;
 (Acetylacetonato-\k^2^<i>O</i>,<i>O</i>')chloridotrimethanolatoniobium(V)
;
_journal_coeditor_code           PV2289
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m801
_journal_page_last               m802
_journal_paper_doi               10.1107/S1600536810021719
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Nb (C H3 O)3 (C5 H7 O2) Cl]'
_chemical_formula_moiety         'C8 H16 Cl Nb O5'
_chemical_formula_sum            'C8 H16 Cl Nb O5'
_chemical_formula_weight         320.57
_chemical_name_systematic
;
(Acetylacetonato-\k^2^<i>O</i>,<i>O</i>')chloridotrimethanolatoniobium(V)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_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_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            8
_cell_length_a                   12.296(5)
_cell_length_b                   12.915(4)
_cell_length_c                   15.470(5)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.64
_cell_volume                     2456.7(15)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type
;
Bruker X8 APEXII 4K Kappa CCD
;
_diffrn_measurement_method       '\w and \f 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  0.0302
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28601
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.8047
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.874
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+3.5334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                2757
_reflns_number_total             3083
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2289.cif
_cod_data_source_block           I
_cod_original_cell_volume        2456.7(16)
_cod_database_code               2226633
_cod_database_fobs_code          2226633